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At least 235 records · Page 13

Thermal fatigue and oxidation data of TAZ-8A and M22 alloys and variations

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.

Hofer, K. E.↗

Ellipsometric study of oxide films formed on LDEF metal samples

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.

Franzen, W.↗

Predicted inlet gas temperatures for tungsten fiber reinforced superalloy turbine blades

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.

Winsa, E. A.↗

Development of W-Ta generator

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.

Source record↗

Triple Layer Tungsten Trioxide, Graphene, and Polyaniline Composite Films for Combined Energy Storage and Electrochromic Applications

Different polyaniline (PANI)-based hybrid films were successfully prepared by electro-polymerizing aniline monomers onto pre-spin-coated indium tin oxide (ITO) glass slides with WO 3 , graphene, or WO 3 /graphene films. Comparing with pristine PANI, the shifts of the characteristic peaks of PANI-based nanocomposites in UV-visible absorption spectra (UV-vis) and Fourier transform infrared spectroscopy (FT-IR) indicate the chemical interaction between the PANI matrix and the nanofillers, which is also confirmed by the scanning electron microscope (SEM) images. Corresponding coloration efficiencies were obtained for the WO 3 /PANI (40.42 cm 2 C -1 ), graphene/PANI (78.64 cm 2 C -1 ), and WO 3 /graphene/PANI (67.47 cm 2 C -1 ) films, higher than that of the pristine PANI film (29.4 cm 2 C -1 ), suggesting positive effects of the introduced nanofillers on the electrochromic performance. The areal capacitances of the films were observed to increase following the order as bare WO 3 < WO 3 /graphene < pristine PANI < WO 3 /PANI < graphene/PANI < WO 3 /graphene/PANI films from both the cyclic voltammogram (CV) and galvanostatic charge-discharge (GCD) results. The enhanced energy storage and electrochromic performances of the PANI-based nanocomposite films can be attributed to the capacitance contributions of the introduced nanofillers, increased PANI amount, and the rougher morphology due to the embedment of the nanofillers into the PANI matrix. This extraordinary energy storage and electrochromic performances of the WO 3 /graphene/PANI film make it a promising candidate for combined electrochromic and energy storage applications.

36 MATERIALS SCIENCE↗

Surface Analysis and Hydrogen Permation Measurements for Super-Permeating Membrane Materials

In this report, we summarize preliminary surface characterization results for Nb surfaces, using low energy ion scattering, direct recoil spectrometry, and Auger electron spectroscopy. While most surface analysis tools cannot detect hydrogen, the low energy ion beam techniques described here are among the few techniques that are directly sensitive to it. For this study, we examined chemisorption using both molecular and atomic hydrogen (using an heated tungsten capillary to dissociate the hydrogen.) To complement these results, we have been performing ex-situ spectroscopic ellipsometry as a means of detecting the surface oxide.

36 MATERIALS SCIENCE↗

Predicted inlet gas temperatures for tungsten fiber reinforced superalloy turbine blades

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.

Winsa, E. A.↗

Xenon-Ion Drilling of Tungsten Films

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.

Garner, C. E.↗

PYROLYTIC GRAPHITE ROCKET THRUST CHAMBER INVESTIGATION PROJECT. MONTHLY LETTER

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.

ROCKET ENGINE↗

Thermophotovoltaic Generators Using Selective Metallic Emitters

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.

Fraas, Lewis M.↗

Stabilization of Tungsten-Uranium Dioxide Composites Under Thermal Cycling Conditions

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.

Gluyas, Richard E.↗

Chemistry effects on ODS steel consolidated via laser powder bed fusion from GARS powder

Oxide Dispersion Strengthened (ODS) steels are promising candidate alloys for structural and cladding applications in extreme environments. They contain a high density of nanoscale oxides for high temperature mechanical strength and radiation resistance. In this work, gas atomization reaction synthesis (GARS) was used to produce powders that were used for additive manufacturing (AM) Laser Powder Bed Fusion consolidation of ODS steels, in order to skip the traditional mechanical alloying of blended yttria and alloy powders. Powder containing iron, chromium, and tungsten with varying amounts of yttrium, titanium, oxygen and zirconium were used to produce ODS steel samples. AM consolidated specimens and powder samples were characterized with transmission electron microscopy. TEM imaging, diffraction patterns, and energy dispersive X-ray spectroscopy (EDS) was used to identify phases present before and after consolidation across chemistries. The effect of the controlled oxygen input (from GARS) and the oxide-forming additions (Y, Ti, Zr) on precipitate size distribution and composition is substantiated and discussed.

36 MATERIALS SCIENCE↗

Electrochemical properties of Gd(III) ions in LiCl-KCl-GdCl 3 at 723–1023 K

Electrochemical behavior of Gd(III) ions in molten LiCl-KCl-GdCl 3 was investigated at 723–1023 K via cyclic voltammetry using tungsten as a working electrode, Gd-Bi (mole fraction, x Gd = 0.16) as a reference electrode, and Gd-Bi (x Gd = 0.02) as a counter electrode. A single reduction–oxidation wave was observed, confirming a single-step, 3-electron transfer Gd(III)/Gd transition. The cathodic peak potential exhibited minimal change (<13 mV) over a wide range of scan rates (0.05–0.30 V s –1 ), indicating facile charge transfer kinetics (i.e., a reversible electrode process). A nucleation overpotential associated with solid Gd deposition was observable at low temperatures (T < 823 K). The mass transport properties of Gd(III) ions were estimated using the Berzins and Delahay relation based on diffusion-limiting peak current. The diffusivity values were determined to be D Gd(III) = 0.5–2.7 × 10 –5 cm 2 s –1 at 723–1023 K with an associated activation energy of E a = 33.9 (±1.0) kJ mol –1 . Finally, the two-phase [liquid + GdBi] Gd-Bi alloy reference electrode experienced less than 0.5 mV of drift over 5 days of repeated electrochemical measurements, indicating high stability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Alloyed coatings for dispersion strengthened alloys

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.

Wermuth, F. R.↗

Investigation of conductive thermal control coatings by a contactless method in vacuo

A technique for determining the conductance per unit area of thermal control coatings for electrostatically clean spacecraft is described. In order to simulate orbital conditions more closely, current-density-voltage (j-V) curves are obtained by a contactless method in which the paint on an aluminum substrate is the anode of a vacuum diode configuration with a tungsten filament cathode. Conductances per unit area which satisfy the International Sun Earth Explorer (ISEE) requirement were observed on black paints containing carbon and in white and green paints filled with zinc oxide which were fired in order to induce defect conductivity. Because of surface effects and the nonhomogeneous nature of paints, large discrepancies were found between measurements with the contactless method and measurements employing metallic contacts, particularly at low current densities. Therefore, measurements with metallic contacts are considered to be of questionable value in deciding the suitability of coatings for electrostatic charge control.

Viehmann, W.↗

Synthesis of LaWN 3 nitride perovskite with polar symmetry

Perovskite structured materials have a variety of uses as photovoltaics, capacitors, and micromechanical actuators, along with other applications. Oxides, halides, and chalcogenides all have large numbers of perovskite structured materials. Examples of perovskite nitrides are conspicuously absent, but Talley et al managed to synthesize one (see the Perspective by Hong). Lanthanum tungsten nitride in the perovskite structure turns out to be piezoelectric, which is ideal for a variety of applications. Perovskite structured nitrides are very attractive because they could easily integrate with the large number of nitride-based semiconducting devices already in use.

36 MATERIALS SCIENCE↗

Development of Coatings for Tantalum Alloy Nozzle Vanes

A group of silicide coatings developed for the T222 tantalum-base alloy have afforded over 600 hours of protection at 1600 and 2400 F during cyclic exposure in air. These coatings were applied in two steps. A modifier alloy was applied by slurry techniques and was sintered in vacuum prior to siliciding by pack cementation in argon. Application of the modifier alloy by pack cementation was found to be much less effective. The addition of titanium and vanadium to molybdenum and tungsten yielded beneficial modifier alloys, whereas the addition of chromium showed no improvement. After siliciding, the 15Ti- 35W-15V-35Mo modifier alloy exhibited the best performance; one sample survived 1064 hours of oxidation at 2400 F. This same coating was the only coating to reproducibly provide 600 hours of protection at both 1600 and 2400 F; in the second and third of three experiments, involving oxidation of three to five specimens at each temperature in each experiment, no failures were observed in 600 hours of testing. The slurry coatings were also shown to protect the Cb752 and D43 columbium-base alloys.

PROTECTIVE COATING↗