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Assessment of grain growth kinetics at temperatures near the melting point and investigation into the use of potential nucleating agents in combination with the naturally occurring BeO led to the definition of critical low-g experiments which would help to determine whether one or both of these possibilities are valid and whether space processing would be able to yield fine grain ingot beryllium.
Volume fraction of a constituent or phase was estimated in six specimens of conventional and DS-eutectic superalloys, using ASTM E562-76, a new standard recommended practice for determining volume fraction by systematic manual point count. Volume fractions determined ranged from 0.086 to 0.36, and with one exception, the 95 percent relative confidence limits were approximately 10 percent of the determined volume fractions. Since the confidence-limit goal of 10 percent, which had been arbitrarily chosen previously, was achieved in all but one case, this application of the new practice was considered successful.
The successful application of high creep strength, directionally solidified gamma/gamma prime-delta (Ni-19.7Cb-6Cr-2.5Al) eutectic superalloy turbine blades requires the development of suitable coatings for airfoil, root and internal blade surfaces. In order to improve coatings for the gamma/gamma prime-delta alloy, the current investigation had the goals of (1) refining promising coating compositions for directionally solidified eutectics, (2) evaluating the effects of coating/ substrate interactions on the mechanical properties of the alloy, and (3) evaluating diffusion aluminide coatings for internal surfaces. Burner rig cyclic oxidation, furnace cyclic hot corrosion, ductility, and thermal fatigue tests indicated that NiCrAlY+Pt(63 to 127 micron Ni-18Cr-12Al-0.3Y + 6 micron Pt) and NiCrAlY(63 to 127 micron Ni-18Cr-12Al-0.3Y) coatings are capable of protecting high temperature gas path surfaces of eutectic alloy airfoils. Burner rig (Mach 0.37) testing indicated that the useful coating life of the 127 micron thick coatings exceeded 1000 hours at 1366 K (2000 deg F). Isothermal fatigue and furnance hot corrosion tests indicated that 63 micron NiCrAlY, NiCrAlY + Pt and platinum modified diffusion aluminide (Pt + Al) coating systems are capable of protecting the relatively cooler surfaces of the blade root. Finally, a gas phase coating process was evaluated for diffusion aluminizing internal surfaces and cooling holes of air-cooled gamma/gamma prime-delta turbine blades.
The oxidation at 900 and 1,000 C of four nickel-base superalloys in 1 atmosphere of slowly flowing oxygen was investigated. Thermogravimetric rate data were obtained for periods to 100 hours. The morphology and composition of the oxide scales formed after 100 hours were studied by optical microscopy, X-ray diffraction, electron microprobe, scanning electron microscopy, and X-ray photoelectron spectroscopy (ESCA). Alloys B-1900 and VIA were found to be primarily alumina formers, though probably 25 percent of their surface was covered by CR2O3-containing oxides at 900 C. Alloys 713C and IN-738 were primarily chromia formers, though the surface of 713C at 1,000 C was covered with NiO, and the surface of IN-738 at both temperatures was covered with a thin layer of TiO2.
High gradient allows rapid growth rates in directionally-solidified eutectic alloys. Furnace design permits cost reductions in directional solidification process through its increased solidification rates, which reduces melt/mold interaction. It produces structural engineering materials for any application requiring properties directionally-solidified eutectic materials.
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The software developed for the solidification model is presented. A link between the calculations and the FORTRAN code is provided, primarily in the form of global flow diagrams and data structures. A complete listing of the solidification code is given.
The operation of solidification model 1 is described. Model 1 calculates the macrosegregation in a rectangular ingot of a binary alloy as a result of horizontal axisymmetric bidirectional solidification. The calculation is restricted to steady-state solidification; there is no variation in final local average composition in the direction of isotherm movement. The physics of the model are given.
The effects of trace metal impurities in coal-derived liquids on deposition, high temperature corrosion and fouling were examined. Alloys were burner rig tested from 800 to 1100 C and corrosion was evaluated as a function of potential impurities. Actual and doped fuel test were used to define an empirical life prediction equation. An evaluation of inhibitors to reduce or eliminate accelerated corrosion was made. Barium and strontium were found to limit attack. Intermittent application of the inhibitors or silicon additions were found to be effective techniques for controlling deposition without losing the inhibitor benefits. A computer program was used to predict the dew points and compositions of deposits. These predictions were confirmed in deposition test. The potential for such deposits to plug cooling holes of turbine airfoils was evaluated. Tests indicated that, while a potential problem exists, it strongly depended on minor impurity variations.
Sputtered coatings of Mo, W, Pt, Ag, Au, Co, Cr, Ni, Ag + Cu, Mo + Pt, Si3N4, A1N, Cr3C2, Ta5Si3, and ZrO2 were applied to a 2-inch-square, 7-inch-long thermal fatigue test specimen which was then internally water cooled and alternately immersed in molten aluminum and cooled in air. After 15,000 cycles the thermal fatigue cracks at the specimen corners were measured. Results indicate that a significant improvement in thermal fatigue resistance was obtained with platinum, molybdenum, and tungsten coatings. Metallographic examination indicates that the improvement in thermal fatigue resistance resulted from protection of the surface of the die steel from oxidation. The high yield strength and ductility of molybdenum and tungsten contributed to the better thermal fatigue resistance.
Three experimental research designs investigating candidate materials and processes involved in protective die surface coating procedures by sputter deposition, using ion beam technologies, are discussed. Various pre-test results show that none of the coatings remained completely intact for 15,000 test cycles. The longest lifetime was observed for coatings such as tungsten, platinum, and molybdenum which reduced thermal fatigue, but exhibited oxidation and suppressed crack initiation only as long as the coating did not fracture. Final test results confirmed earlier findings and coatings with Pt and W proved to be the candidate materials to be used on a die surface to increase die life. In the W-coated specimens, which remained intact on the surface after thermal fatigue testing, no oxidation was found under the coating, although a few cracks formed on the surface where the coating broke down. Further research is planned.
New technique converts finely powdered silicon into solid pellets. Fine silicon powder melts in thin quartz bubble that breaks upon cooling, leaving behind crack-free pellet of silicon.
Directional solidification by the Heat Exchanger Method (HEM) is a viable approach for directional solidification of silicon ingots used for terrestrial solar cell applications. Some of the significant advances made during this phase of the program were: ingot size, 34 cm x 34 cm x 17 cm - 45 kg, usable material yield - 90%, solar cell efficiency averaged over the whole ingot - 85% of control CZ (35 kg ingot), very uniform resistivity over the boule, and cycle time for 36 kg ingots - 56 hours. Some of the problems encountered were growth rate decrease with increased ingot height, silicon carbide precipitates, and high dislocation density in HEM material. The silicon carbide is attributed to backstreaming of oil vapors from the vacuum pump; the high dislocation density is associated with the thermal history of the boule.
The effects of Cr, Al, Ti, Mo, Ta, Nb, and W content on the hot corrosion of nickel base alloys were investigated. The alloys were tested in a Mach 0.3 flame with 0.5 ppmw sodium at a temperature of 900 C. One nondestructive and three destructive tests were conducted. The best corrosion resistance was achieved when the Cr content was 12 wt %. However, some lower-Cr-content alloys ( 10 wt%) exhibited reasonable resistance provided that the Al content alloys ( 10 wt %) exhibited reasonable resistance provided that the Al content was 2.5 wt % and the Ti content was Aa wt %. The effect of W, Ta, Mo, and Nb contents on the hot-corrosion resistance varied depending on the Al and Ti contents. Several commercial alloy compositions were also tested and the corrosion attack was measured. Predicted attack was calculated for these alloys from derived regression equations and was in reasonable agreement with that experimentally measured. The regression equations were derived from measurements made on alloys in a one-quarter replicate of a 2(7) statistical design alloy composition experiment. These regression equations represent a simple linear model and are only a very preliminary analysis of the data needed to provide insights into the experimental method.