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Applications and limitations of proposed concept of effective binary diffusion coefficient for analyzing interdiffusion of multicomponent systems
Interdiffusion in rhenium emitters fabricated by pressure bonding tested with electron beam, discussing thermal cycling effect
Investigating interdiffusion of W-Ta, W-Mo, and W-Nb systems in refractory temperature range
Refractory metal thermionic emitter-support systems, measuring surface interdiffusion at high temperatures
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.
Cyclic furnace oxidation studies were conducted on the cobalt alloy WI-52 clad with Ni-30Cr, Fe-25Cr-4A1, and Ni-20Cr-4A1 foils (0.051 to 0.254 mm thick). Tests as long as 400 hours using 1- and 20-hour cycles showed that the Ni-Cr- and Fe-Cr-A1 claddings were about equally protective at both temperatures. The protective ability of these alloys was influenced by exposure temperature and cladding thickness. At both temperatures, they protected WI-52 about as well as, or better than, a widely used commercial aluminide coating. The Ni-Cr-Al claddings did not protect WI-52 nearly as well. Interdiffusion generally influenced the oxidation behavior of all clad WI-52 systems.
Diffusion coefficients have been measured for Cr51 in fine- and coarse-grained TDNiCr (Ni-20Cr-2ThO2) and in fine-grained Ni-20Cr in the temperature range from 1038 to 1200 C. Selective diffusivities have also been determined for specimens of these alloys which were aluminized to give an initial surface concentration of 5.8 wt % Al. Finally, diffusion coefficients for interdiffusion of aluminum in TDNiCr and Ni-20Cr have been obtained from electron probe microanalysis of the aluminized specimens. For a given grain size and temperature there is no difference in diffusivities for chromium diffusion in TDNiCr or Ni-20Cr. Diffusion coefficients increase with decreasing grain size for both alloys. Comparison of aluminum diffusion data obtained from electron microprobe profiles with radiotracer chromium diffusivities suggests that aluminum diffuses approximately three times faster than chromium in TDNiCr and Ni-20Cr.
Experiments were performed to critically demonstrate the effects of diffusion on the aluminum depletion and degradation of NiAl coatings on superalloys. Pack aluminized IN 100 and Mar-M200 were diffusion annealed in 0.0005 torr vacuum at 1100 C for 300 hours. Aluminum losses due to oxidation and vaporization were minimal. Metallographic and electron microprobe analyses showed considerable interdiffusion of the coating with the substrate, which caused a large decrease in the original aluminum level of the coating. Subsequent cyclic furnace oxidation tests were performed at 1100 C using 1 hour cycles on pre-diffused and as-coated specimens. The pre-diffusion treatment decreased the oxidation protection for both alloys, but more dramatically for IN 100. Identical oxidation tests of bulk NiAl, where such diffusion effects are precluded, showed no signs of degradation at twice the time needed to degrade the coated superalloys.
Improved aluminide/barrier coating combinations for dispersion strengthened nickel materials were investigated. The barrier materials involved alloys with refractory metal content to limit interdiffusion between the coating and the substrate, thereby minimizing void formation. Improved aluminide coatings involved the dispersion of aluminum-rich compounds. Coatings were tested in argon at 1533 K (2300 F) for 100 hours and in cyclic oxidation at 1422 K (2100 F). Two coatings on TDNiCr completed 300 hours of oxidation testing, none on TDNi. Selected coating combinations were evaluated in Mach 1 burner rig testing using JP-4 fuel and air at 1422 K (2100 F) and 1477 K (2200 F) for 350 and 100 hours, respectively. Static oxidation in 1-hour cycles was conducted at 1533 K (2300 F) for 100 hours. For comparison purposes a physical vapor deposition (PVD) NiCrAlY coating was tested concurrently. Only the NiCrA1Y coating survived the 1477 K (2200 F)/100-hour burner rig test and 275 hours of the 350-hour 1422 K (2100 F) test. Elevated temperature exposure reduced room temperature tensile properties but had little effect on elevated temperature properties.
The interdiffusion of platimum and gold films, a couple utilized in beam lead microcircuits, has been studied for temperatures up to 550 C. Gold-on-platinum couples and separate platimum and gold films 80-450 nm thick, were deposited by electron beam evaporation onto oxidized (111) silicon substrates. Diffusion was monitored by means of spectral reflectance versus wavelength in the band 500-1000 nm. The separate metal films showed good adhesion and stable reflectances (after an initial change) for at least 6 h at diffusion temperatures, in contrast to the couples. Analysis of platinum diffusion through the gold films yielded an activation energy about 38 kcal/g-atom and a pre-exponential factor of the order 0.001 sq cm/sec, values close to those for volume diffusion. The pre-exponential factor especially is dependent upon film deposition conditions.
In situ nucleation and growth measurements of Ag and Au on single-crystal PbSe thin films were made using a transmission electron microscope. Properties studied were polymorphism, crystalline perfection, and the stoichiometric composition of the initial and the autoepitaxially thickened PbSe substrates. The quantitative nucleation and cluster growth measurements were limited to low-saturation conditions. The epitaxial orientations are discussed, and evidence is presented as to the stage of deposition at which the epitaxial order for Ag is introduced. Strong substrate/overgrowth interaction manifested itself by alloying and interdiffusion.
Experiments were performed to critically demonstrate the effects of diffusion on the aluminum depletion and degradation of NiAl coatings on superalloys. Pack aluminized IN 100 and Mar-M200 were diffusion annealed in 5 mtorr vacuum at 1100 C for 300 hr. Aluminum losses due to oxidation and vaporization were minimal. Metallographic and electron microprobe analyses showed considerable interdiffusion of the coating with the substrate, which caused a large decrease in the original aluminum level of the coating. Subsequent cyclic furnace oxidation tests were performed at 1100 C using 1 hr cycles on prediffused and as-coated specimens. The prediffusion treatment decreased the oxidation and as-coated specimens. The prediffusion treatment decreased the oxidation protection for both alloys, but more dramatically for IN 100. Identical oxidation tests of bulk NiAl, where such diffusion effects are precluded, showed no signs of degradation at twice the time needed to degrade the coated superalloys.
The behavior of Ti-Mo-Au metallization on Al2O3 and C has been investigated by backscattering spectrometry. Results show that Mo-Au bimetal films typically mix during deposition. Diffusion of Ti in Mo film occurs at 600 C, but is inhibited by the presence of oxygen in the Ti film. Even 1000 A of Mo is not a barrier against interdiffusion of Ti and Au during 20-min anneals at 600 C. The amount of mixing observed also depends on the nature of the substrate which supports the Ti-Mo-Au metallization.
A chemical compatibility study was conducted between SiC filament and the following P/M matrix alloys: Waspaloy, Hastelloy-X, NiCrAlY, Ha-188, S-57, FeCrAlY, and Incoloy 800. None of the couples demonstrated sufficient chemical compatibility to withstand the minimum HIP consolidation temperatures (996 C) or intended application temperature of the composite (982 C). However, Waspaloy, Haynes 188, and Hastelloy-X were the least reactive with SiC of the candidate alloys. Chemical vapor deposited tungsten was shown to be an effective diffusion barrier between the superalloy matrix and SiC filament providing a defect-free coating of sufficient thickness. However, the coating breaks down when the tungsten is converted into intermetallic compounds by interdiffusion with matrix constituents. Waspaloy was demonstrated to be the most effective matrix alloy candidate in contact with the CVD tungsten barrier because of its relatively low growth rate constant of the intermediate compound and the lack of formation of Kirkendall voids at the matrix-barrier interface. Fabrication methods were developed for producing panels of uniaxial and angle ply composites utilizing CVD tungsten coated filament.
The equilibrium stability criterion for diffuse interfaces in a two-component solution with a miscibility gap requires that the interdiffusion flux vanish. If the system is continuously deformed, convective fluxes disrupt the equilibrium in the interface regions and induce a counter diffusive flux, which is dissipative and contributes to the apparent viscosity of the mixture. Chemical free energy is recoverably stored, causing viscoelastic phenomena. Both effects are significant.
Microscopic aspects of interfacial reactions are discussed, such as interdiffusion, formation of intermetallic phases, generation and annihilation of lattice defects, effect of temperature, grain size, etc., which normally occur in diffusion bonding processes. Relationships between properties and microstructure in thin film couples are examined utilizing a unique combination of contact resistance measurements and characterization by transmission electron microscopy.
The flight test furnace run of the monotectic and syntectic alloys experiment was successfully performed during the Apollo-Soyuz Test Project mission in July 1975. Examination of the returned sample cartridges and the formal comparative characterization of the low-g and one-g processed samples of lead-zinc and aluminum antimonide were completed. The results for aluminum antimonide show that polycrystalline and multiphased material can be homogenize in space under low-g conditions. Microstructural study on the lead-zinc flight samples shows that complete interdiffusion of lead and zinc had not been achieved, even though the flight data indicated a soak temperature in the miscible region that was 40 K above the published consolute temperature.
The formation of voids through interdiffusion in bimetallic welded structures exposed to high operating temperatures is inhibited by utilizing an alloy of the parent materials in the junction of the parent materials or by preannealing the junction at an ultrahigh temperature. These methods are also used to reduce the concentration gradient of a hardening agent.