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Inverted Bridgman Method yields crystals of higher homogeneity and better structure than those grown by ordinary Bridgman method. Process controls thermotransport by holding molten alloy in known temperature for known period of time. Rapid cooling quenches in state of segregation. Method is applicable to other eutectiferous systems where thermotransport is appreciable.
A nominal composition of Co-15Cr-20Ni-10.5Hf-0.7C was directionally solidified at 0.8 cm/hr growth rate to produce aligned HfC in a cobalt matrix alloy. The aligned HfC fibers were present as rod and plate types. The diameter of the aligned fibers was about 1 micron, with volume fraction in the range of 11 to 15 per cent. The growth direction of the fibers was parallel to the 100 direction. The alloy was subjected to thermal cycling between 425 and 1100 C, using a 2.5 minute cycle. No microstructural degradation of the HfC fibers in the alloy was observed after 2500 cycles.
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Quaternary modifications and quinary additions from the elements Co, Ti, Mo, W, Re, B, Si, and Ta to the baseline quaternary alloy gamma/gamma prime-delta Ni-19.7 at.% Nb-6.0 at.% Cr-2.5 at.% Al are examined for various concentrations. From modification studies five alloys were chosen for detailed mechanical property characterization: Ni-19.7 Nb-6.0 Cr-2.5 Al-1.0 W; Ni-19.7 Nb-6.0 Cr-2.5 Al-1.0 Mo; Ni-18.6 Nb-6.0 Cr-2.5 Al-0.87 Ti; Ni-20.2 Nb-6.0 Cr-2.5 Al-2.0 Co; and Ni-17.9 Nb-6.0 Cr-2.5 Al-3.0 Ta. It is shown that extensive alloying of the baseline quaternary alloy is possible for elements exhibiting a wide solubility range in both phases, and that limited substitution of W, Mo, Re, Si, and B is possible for elements with restricted solid solubility especially in the delta phase. Improvement of creep rupture strength and cyclic oxidation resistance at 1100 C is discussed.
The construction of a solar furnace was completed and it was tested after a preliminary alignment of the heliostat mirrors. After final alignment, the solar furnace is used for directional solidification experiments designed to simulate space conditions.
Ingots of Pb-61.9 Sn were undercooled and solidified under increasing gravity levels in order to investigate the effects of segregation. The onset of convective flow subsequent to the nucleation of lead is demonstrated. It is shown that when material system in the molten state contains constituents of varying densities, the combination of gravitational forces on the nucleating species and the amount of undercooling of the melt will determine the resultant segregation.
Thermal fatigue and oxidation data were obtained on 61 specimens, representing 15 discrete alloy compositions or fabricating techniques and three coating systems. Conventionally fabricated alloys included V57, MM 200, Rene 77, Rene 125, MM 246, MM 509, IN-738, IN-792 + Hf, and MM 200 + Hf. The directionally solidified alloys were MM 200, MM 200 single crystal, MM 200 bicrystal, cellular gamma/gamma' - delta) and lamellar gamma/gamma' - delta. The coatings systems included NiCrAlY on IN-738, In-792 + Hf, MM 200 DS, MM 200 DS single crystal, and cellular gamma/gamma' - delta and NiCrAlY/Pt on lamellar gamma/gamma' - delta. Crack initiation survival rates were recorded for all alloys, with and without coatings. All uncoated alloys, except MM 509, exhibited significant oxidation weight loss in 75,000 to 15,000 cycles. MM 509 specimens had weight losses only slightly higher than coated specimens through 7,500 cycles. All coated specimens had low weight loss.
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Directionally solidified Mo alloys are evaluated to determine the shear rupture strength and to possibly improve it by microstructural and heat treatment variations. Bars of the alloy containing nominally 5.7% Al and 33.5% Mo by weight with balance Ni were directionally solidified at rates between 10 and 100 mm per hour in furnaces with thermal gradients at the liquid-solid interface of 250 or 100 C per cm. A limited number of longitudinal shear rupture tests were conducted at 760 C and 207 MPa in the as - solidified and in several heat treated conditions. It is shown that shear rupture failures are partly transgranular and that resistance to failure is prompted by good fiber alignment and a matrix structure consisting mainly of gamma prime. Well aligned as - solidified specimens sustained the shear stress for an average of 81 hours. A simulated coating heat treatment appeared to increase the transformation of gamma to gamma prime and raised the average shear life of aligned specimens to 111 hours. However, heat treatments at 1245 C and especially at 1190 C appeared to be detrimental by causing partial solutioning of the gamma prime, and reducing lives to 47 and 10 hours, respectively.
Alloys from the following systems were selected for property evaluation: (1) gamma/gamma-Mo (Ni-base, rods of Mo); (2) gamma-beta (Ni-base, lamellae or rods of (Ni, Fe/Co Al); and (3) gamma-gamma (Ni-base rods of Ni3Al gamma). The three alloys were subjected to longitudinal and transverse tensile and rupture tests from 750 C to 1100 C, longitudinal shear strength was measured at several temperatures, resistance to thermal cycling to 1150 C was determined, cyclic oxidation resistance was evaluated at 750 C and 1100 C, and each system was directionally solidified in an alumina shell mold turbine shape to evaluate mold/metal reactivity. The gamma/gamma Mo system has good rupture resistance, transverse properties and processability, and is a high potential system for turbine blades. The gamma-beta system has good physical properties and oxidation resistance, and is a potential system for turbine vanes. The gamma-gamma system has good high temperature rupture resistance and requires further exploratory research.
A simple ternary gamma/gamma-prime-alpha alloy of nominal composition (wt-%) Ni-32Mo-6Al has been directionally solidified at 17 mm/h and tested in creep rupture at 1073, 1173, and 1273 K. A uniform microstructure consisting of square-shaped Mo fibers in a gamma + gamma-prime matrix was found despite some variation in the molybdenum and aluminum concentrations along the growth direction. Although the steady-state creep rate is well described by the normal stress temperature equation, the stress exponent (12) and the activation energy (580 kJ/mol) are high. The rupture behavior is best characterized by the Larson-Miller parameter where the constant equals 20.
Iron base alloys containing aluminum and chromium together with smaller amounts of yttrium and silicon are of interest for high temperature applications. Strengthening an inherently weak but oxidation resistant solid solution matrix with aligned in situ chromium carbides represents an attractive approach to achieving both surface stability and creep resistance at elevated temperatures. Aligned microstructures were produced in alloys of approximately 30 wt % (Cr + Mn), about 3 wt % C and the balance Fe consisting of a gamma matrix and the hexagonal carbide (Cr, Mn, Fe)7C3. The tensile and stress rupture strength to 2000 F of aligned Fe-20 w/t % Cr-10 wt % Mn-3.2 wt % C measured parallel to the carbide reinforcement exceeded those of the strongest iron-nickel superalloys, e.g., CRM-6D developed by Chrysler for automotive turbine application. The cyclic oxidation and sulfidation response of these alloys at elevated temperatures can be markedly improved by aluminum additions.
For the quasi-regular fibrous microstructure of MnBi formed at freezing rates of 9 mm/h and above, good agreement between experimental and theoretical results for fiber spacing, freezing rate, radial position, and ampoule rotation rate is found. For the irregular blade-like microstructure formed at lower freezing rates, convection is found to coarsen the microstructure somwhat more than predicted. The volume fraction of MnBi was also shown to depend on ampoule rotation and radial position, even in the absence of ampoule rotation. The two-fold finer microstructure observed in space-processed material could not be explained by the elimination of buoyancy-driven natural convection.
Convection was generated during directional solidification by the accelerated crucible rotation technique (spin up/spin down). This stirring increased the rotation rate of the microstructure and reduced the length solidifying cooperatively, but had no influence on the lamellar spacing.
Alloy compositions centering about Sn- 5 to 15 wt pct Al and Pb- 4 to 20 wt pct Cu have been directionally solidified as a function of growth rate and orientation with respect to earth's gravity vector. The effect of these processing variables on macrosegregation is presented, and the consequence of a structural transition from primary columnar to equiaxed dendritic growth is examined. Effects detrimental to microstructure and attributed to density variations are shown to be minimized by a novel processing technique. In view of the ground-based results, some considerations follow regarding what might be gained by solidifying these alloys in a microgravity environment.
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Partitioning coefficients for metal/sulfide liquid, troilite/sulfide liquid, and schreibersite/sulfide liquid were determined for Ag, Au, Mo, Ni, Pd, and Tl (using EMPA and proton-induced X-ray microprobe and ion microprobe analyses) in order to understand the chronometer systems of iron meteorites. In general, the obtained schreibersite/metal and troilite/metal partition coefficients for 'compatible' elements were quite similar to those inferred from natural assemblages, reinforcing an earlier made conclusion that there is a class of elements for which experimental troilite/metal and schreibersite/metal partition coefficients approximate those inferred from natural samples. The consistency between experimental and natural assemblages, however, was not observed for Ag, Pb, and Tl, indicating that the abundances of these elements determined in 'metal' and 'troilite' separates from iron meteorites are influenced by trace minerals that concentrate incompatible elements.