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NiCrAl alloys are improved by the addition of zirconium. These alloys are in the Beta or gamma/gamma' + Beta region of the ternary system. Zirconium is added in a very low amount between 0.06 and 0.20 weight percent. There is a narrow optimum zirconium level at the low value of 0.13 weight percent. Maximum resistance to cyclic oxidation is achieved when the zirconium addition is at the optimum value.
Thermal gradient testing of three oxide dispersion strengthened alloys (two Ni-base alloys, MA 754 and MA 6000 E, and the Fe-base MA 956) and the directionally solidified eutectic alloy, gamma/gamma prime-alpha, have been conducted. Experiments were carried out with maximum temperatures up to 1200 C and thermal gradients on the order of 100 C/mm. The oxide dispersion strengthened alloys were difficult to test because the thermal stresses promoted crack nucleation and growth; thus the ability of these alloys to maintain a thermal gradient may be limited. The stability of individual fibers in gamma/gamma prime-alpha was excellent; however, microstructural changes were observed in the vicinity of grain boundaries. Similar structures were also observed in isothermally annealed material; therefore thermal gradients do not affect the microstructure of gamma/gamma prime-alpha in any significant manner.
The thermal fatigue resistance of several oxide dispersion strengthened (ODS) alloys has been evaluated through cyclic exposure in fluidized beds. The ODS nickel-base alloy MA 754 and ODS iron-base alloy MA 956 as well as four experimental ODS Ni-16Cr-4.5Al base alloys with and without Ta additions were examined. Both bare and coated alloys were subjected to up to 6000 cycles where each cycle consisted of a 3 minute immersion in a fluidized bed at 1130 C followed by a 3 minute immersion in a bed at 357 C. Testing revealed that the thermal fatigue resistance of the ODS nickel-base alloys was excellent and about equal to that of directionally solidified superalloys. However, the thermal fatigue resistance of MA 956 was found to be poor. Metallographic examination of tested specimens revealed that, in general, the post-test microstructures can be rationalized on the basis of previous diffusion, mechanical property, and oxidation studies.
Ternary Co-Cr-Al alloy oxidation data, detailing kinetics, products, mechanisms, resistance behavior and rate
High strength nickel base alloy with improved oxidation resistance up to 2200 degrees F for applicability to gas turbine engine components
High temperature creep behavior of recrystallized nickel-thorium oxide alloys studied with vacuum constant-stress creep conditions
This paper examines results with cyclic oxidation tests of Ni(9-20) Cr(15-30) Al-(x)Zr alloys carried out at 1100 C and 1200 C in static air. The concentration of zirconium varies from 0 to 0.63 atomic percent. Significant aluminum penetration is found in metallographic and electron microscopic examination of oxidized surfaces. Small amounts of zirconium lead to minimal penetration, and with increased zirconium content pronounced oxide penetration is observed.
High tensile strength nickel base alloy with improved oxidation resistance up to 2200 degrees Farenheit
The results of a study conducted to determine the role space processing or materials research in space plays in the superconductor and electrical contact industries are presented. Visits were made to manufacturers, users, and research organizations connected with these products to provide information about the potential benefits of the space environment and to exchange views on the utilization of space facilities for manufacture, process development, or research. In addition, space experiments were suggested which could result in improved terrestrial processes or products. Notable examples of these are, in the case of superconductors, the development of Nb-bronze alloys (Tsuei alloys) and, in the electrical contact field, the production of Ag-Ni or Ag-metal oxide alloys with controlled microstructure for research and development activities as well as for product development. A preliminary experimental effort to produce and evaluate rapidly cooled Pb-Zn and Cu-Nb-Sn alloys in order to understand the relationship between microstructure and superconducting properties and to simulate the fine structure potentially achievable by space processing was also described.
A survey is presented of the cyclic furnace and burner rig oxidation facilities at NASA-Lewis Research Center together with a review of selected test results and an initial interpretation of the data obtained. Cyclic furnace tests are used to conveniently screen alloy oxidation resistance and spall tendency; high velocity tests further indicate dynamic environmental resistance. Alloys which form scales predominantly of Cr2O3/chromite spinel spall much more than those forming alpha Al2O3/aluminate spinel scales. Weight changes due to scale spalling were used to estimate alloy depletion/thickness losses.
The structure of transient scales formed on pure and Y or Zr-doped Ni-15Cr-13Al alloys oxidized for 0.1 hr at 1100 C was studied by the use of transmission electron microscopy. Crystallographically oriented scales were found on all three alloys, but especially for the Zr-doped NiCrAl. The oriented scales consisted of alpha-(Al,Cr)2O3, Ni(Al,Cr)2O4 and gamma-Al2O3. They were often found in intimate contact with each other such that the close-packed planes and directions of one oxide phase were aligned with those of another. The prominent structural features of the oriented scales were approximately equal to micrometer subgrains; voids, antiphase domain boundaries and aligned precipitates were also prevalent. Randomly oriented alpha-Al2O3 was also found and was the only oxide ever observed at the immediate oxide metal interface. These approximately 0.15 micrometer grains were populated by intragranular voids which decreased in size and number towards the oxide metal interface. A sequence of oxidation was proposed in which the composition of the growing scale changed from oriented oxides rich in Ni and Cr to oriented oxides rich in Al. At the same time the structure changed from cubic spinels to hexagonal corundums with apparent precipitates of one phase in the matrix of the other. Eventually randomly oriented pure alpha-Al2O3 formed as the stable oxide with an abrupt transition: there was no gradual loss of orientation, no gradual compositional change or no gradual decrease in precipitate density.
High strength nickel base alloy with improved oxidation resistance up to 2200 degrees F for applicability to gas turbine engine components
Thermal fatigue and oxidation data were obtained 24 specimens representing 9 discrete oxide dispersion-strengthened alloy compositions or fabricating techniques. Double edge wedge specimens, both bare metal and coated for each systems, were cycled between fluidized beds maintained at 1130 C with a three minute immersion in each bed. The systems included alloys identified as 262 in hardness of HRC 38; 264 in hardness of HRC 38, 40 and 43; 265 HRC 39, 266 of HRC 37 and 40; 754; and 956. Specimens in the bare condition of 265 HRC 39 and 266 HRC 37 survived 6000 cycles without cracking on the small radius of the double edge wedge specimen. A coated specimen of 262 HRC 38, 266 HRC 37 and 266 HRC40 also survived 6000 cycles without cracking. A duplicate coated specimen of 262 HRC 38 alloy survived 5250 cycles before cracks appeared. All the alloys showed little weight change compared compared to alloys tested in prior programs.
The effect of the gaseous corrodent NaCl on the high temperature oxidation and sodium sulfate induced hot corrosion behavior of alumina formers, chromia formers, and the superalloy B-1900 was examined. Isothermal experiments were conducted at 900 C and 1050 C in air in the presence and absence of NaCl vapors. Microstructural changes in oxide morphology and increased rates of oxidation were observed when NaCl(g) was present. It is hypothesized that the accelerated rates of oxidation are the result of removal of aluminum from the scale substrate interface and the weakening of the scale substrate bonds. The aluminum removed was redeposited on the surfaces in the form of alumina whiskers. For the superalloy B-1900, alumina whiskers are also formed, and the alloy oxidizes at catastrophic rates. In the case of Ni-25Cr alloy, NaCl vapors interact with the scale depleting it of chromium.
An initial investigation was conducted to determine the effect of platinum addition on the activities of aluminum and nickel in beta-NiAl(Pt) over the temperature range 1354 to 1692 K. These measurements were made with a multiple effusion-cell configured mass spectrometer (multi-cell KEMS). The results of this study show that Pt additions act to decreased alpha(Al) and increased the alpha(Ni) in beta-NiAl(Pt) for constant X(sub Ni)/X(sub Al) approx. = 1.13, while at constant X(sub Al) the affect of Pt on Al is greatly reduced. The measured partial enthalpies of mixing indicate Al-atoms have a strong self interaction while Ni- and Pt-atoms in have similar interactions with Al-atoms. Conversely the binding of Ni-atoms in beta-NiAl decreases with Pt addition independent of Al concentration. These initial results prove the technique can be applied to the Ni-Al-Pt system but more activity measurements are required to fully understand the thermodynamics of this system and how Pt additions improved the scaling behavior of nickel-based superalloys. In addition, with the choice of a suitable oxide material for the effusion-cell, the "closed" isothermal nature of the effusion-cell allows the direct investigation of an alloy-oxide equilibrium which resembles the "local-equilibrium" description of the metal-scale interface observed during high temperature oxidation. It is proposed that with an Al(l) + Al2O3(s) experimental reference state together with the route measurement of the relative partial-pressures of Al(g) and Al2O(g) allows the activities of O and Al2O3 to be determined along with the activities of Ni and Al. These measurements provide a direct method of investigating the thermodynamics of the metal-scale interface of a TGO-scale.
Nickel-rich alloys in the Ni-Cr-Al system were evaluated for cyclic oxidation resistance in still air at 1,100 and 1,200 C. A first approximation oxidation attack parameter Ka was derived from specific weight change data involving both a scaling growth constant and a spalling constant. An estimating equation was derived with Ka as a function of the Cr and Al content by multiple linear regression and translated into countour ternary diagrams showing regions of minimum attack. An additional factor inferred from the regression analysis was that alloys melted in zirconia crucibles had significantly greater oxidation resistance than comparable alloys melted otherwise.
Cobalt chromium high temperature oxidation and scale formation
Viable processes were developed for secondary working of oxide dispersion strengthened (ODS) alloys to near-net shapes (NNS) for aircraft turbine vanes. These processes were shown capable of producing required microstructure and properties for vane applications. Material cost savings of 40 to 50% are projected for the NNS process over the current procedures which involve machining from rectangular bar. Additional machining cost savings are projected. Of three secondary working processes evaluated, directional forging and plate bending were determined to be viable NNS processes for ODS vanes. Directional forging was deemed most applicable to high pressure turbine (HPT) vanes with their large thickness variations while plate bending was determined to be most cost effective for low pressure turbine (LPT) vanes because of their limited thickness variations. Since the F101 LPT vane was selected for study in this program, development of plate bending was carried through to establishment of a preliminary process. Preparation of ODS alloy plate for bending was found to be a straight forward process using currently available bar stock, providing that the capability for reheating between roll passes is available. Advanced ODS-NiCrAl and ODS-FeCrAl alloys were utilized on this program. Workability of all alloys was adequate for directional forging and plate bending, but only the ODS-FeCrAl had adequate workability for shaped preform extrustion.