Raghavan Ayer

The influence of yttrium on oxide scale growth and adherence

Alloys and coatings for high-temperature service are designed to form selectively chromia scales, alumina scales, or, to a limited extent, silica scales upon exposure to the environment. For such oxide scales to be protective, they should be both slow growing and adherent. It turns out that the addition of yttrium to such alloys can often impart both characteristics to the oxide scale. However, the actual operating mechanisms continue to be a matter of controversy among researchers in the area of oxidation. In the present study, the growth and adherence of alumina and chromia scales on alloys containing yttrium, either as an oxide dispersion or as an intermetallic phase, have been investigated in conjunction with detailed oxide scale characterization using the techniques of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and secondary ion mass spectrometry (SIMS). The results of the study are used for critical assessment of the proposed mechanisms, especially the more recent ones, and to suggest some new mechanisms for adherence.

Microanalytical study of the heterogeneous phases in commercial Al-Zn-Mg-Cu alloys

X-ray microanalysis and Convergent Beam Diffraction (CBD) studies were conducted on the second phase constituent and dispersoid particles in 7075 and 7475 aluminum alloys. Partial substitution of alloying elements was found to occur in all the second phase particles causing small deviations from the stoichiometric compositions reported for the binary and ternary compounds. The coarse constituent phases were identified to be Al7Cu2Fe, (Al,Cu)6(Fe,Cu), Mg2Si, α-Al12Fe3Si, amorphous silicon oxide, and a modified Al6Fe compound in decreasing order of abundance. The dispersoid particles were Al18Mg3Cr2 compound, and they formed in both triangular and spherical morphologies. Their compositions were found to vary slightly with the aging treatment. The crystal structure of the dispersoid phase consisted of a disordered form of a cubic structure (Fd3m) reported for the Al18Mg3Cr2 compound. The uniqueness of CBD analysis in the crystal structure determination is emphasized.

Microstructural basis for the effect of chromium on the strength and toughness of AF1410-based high performance steels

The variation in strength and Charpy impact toughness as a function of tempering temperature in the range of 200 ‡C to 650 ‡C was investigated in AF 1410 and AF 1410 + 1 pct Cr steels produced in a laboratory-scale, and a commercially produced AerMet 100 steel. The tensile test results showed that AF 1410 + 1 pct Cr had lower strength compared to AF 1410, while AerMet 100 had the highest strength of the three steels examined. Transmission electron microscopy (TEM) studies demonstrated that the strength variations among the steels can be attributed to differences in the matrix/carbide coherency strain and the volume fraction of the strengthening M2C carbides. The toughness values of the three steels were comparable when tempered up to 424 ‡C. Tempering at and above 454 ‡C resulted in a relative enhancement of toughness in AF 1410 + 1 pct Cr steel compared to AF 1410. This toughening was attributed to the destabilization of cementite at lath and prior austenite boundaries and the formation of reverted austenite.

Instabilities in stabilized austenitic stainless steels

The effect of aging on the precipitation of grain boundary phases in three austenitic stainless steels (AISI 347, 347AP, and an experimental steel stabilized with hafnium) was investigated. Aging was performed both on bulk steels as well as on samples which were subjected to a thermal treatment to simulate the coarse grain region of the heat affected zone (HAZ) during welding. Aging of the bulk steels at 866 K for 8000 hours resulted in the precipitation of Cr23C6 carbides, σ, and Fe2Nb phases; the propensity for precipitation was least for the hafnium-stabilized steel. Weld simulation of the HAZ resulted in dissolution of the phases present in the as-received 347 and 347AP steels, leading to grain coarsening. Subsequent aging caused extensive grain boundary Cr23C6 carbides and inhomogeneous matrix precipitation. In addition, steel 347AP formed a precipitate free zone (PFZ) along the grain boundaries. The steel containing hafnium showed the best microstructural stability to aging and welding.

Phase transformations at steel/IN626 clad interfaces

The microstructures of 4130 and 2.25Cr-1Mo steels clad to nickel base IN625 by welding and HIPing were examined by Analytical Electron Microscopy (AEM) and Secondary Ion Mass Spectroscopy (SIMS) to determine the interfacial microstructural characteristics which could affect their mechanical properties and corrosion resistance. The interface microstructures of the clads produced by the two methods were considerably different. The clad produced by welding was characterized by a low density of carbide precipitates confined to a very narrow region (∼1 μm) at the interface of ferrite and austenite. In addition, a thin region of untempered martensite was present at the interface which could affect its resistance to hydrogen embrittlement as well as other mechanical properties. The interface of the HIP clad composite contained several regions of distinct microstructural characteristics with widely varying densities of carbide precipitates. Relative to the clad produced by welding, extensive precipitation was observed both in the steel and in the IN625 at the interface, separated by a region free from precipitation. The extent of precipitation at the interface regions appears to be controlled essentially by the extent of carbon transport across the interface. The article describes the detailed analysis of the interface characteristics, and models are proposed to explain the microstructural evolution at the interface of the HIP and weld clad composites.

Microstructural characterization of the dispersed phases in Al-Ce-Fe system

Analytical electron microscopy studies were conducted on a rapidly solidified Al-8.8Fe-3.7Ce alloy and arc melted buttons of aluminum rich Al-Fe-Ce alloys to determine the characteristics of the metastable and equilibrium phases. The rapidly solidified alloy consisted of binary and ternary metastable phases in the as-extruded condition. The binary metastable phase was identified to be Al6Fe, while the ternary metastable phases were identified to be Al10Fe2Ce and Al20Fe5Ce. The Al20Fe5Ce was a decagonal quasicrystal while the Al10Fe2Ce phase was determined to have an orthorhombic crystal structure belonging to space group Cmmm, Cmm2, or C222. Microscopy studies of RS alloy and cast buttons annealed at 700 K established the equilibrium phases to be Al13Fe4, Al4Ce, and an Al13Fe3Ce ternary phase which was first identified in the present study. The crystal structure of the equilibrium ternary phase was determined to be orthorhombic with a Cmcm or Cmc2 space group. The details of X-ray microanalysis and convergent beam electron diffraction analysis are described.

Microstructure and Hydrogen-Induced Failure Mechanisms in Fe and Ni Alloy Weldments

The microstructure and fracture morphology of AISI 8630-IN625 and ASTM A182-F22-IN625 dissimilar metal weld interfaces were compared and contrasted as a function of postweld heat treatment (PWHT) duration. For both systems, the microstructure along the weld interface consisted of a coarse grain heat-affected zone in the Fe-base metal followed by discontinuous martensitic partially mixed zones and a continuous partially mixed zone on the Ni side of the fusion line. Within the partially mixed zone on the Ni side, there exists a 200-nm-wide transition zone within a 20-μm-wide planar solidification region followed by a cellular dendritic region with Nb-Mo–rich carbides decorating the dendrite boundaries. Although there were differences in the volume of the partially mixed zones, the major difference in the metal weld interfaces was the presence of M7C3 precipitates in the planar solidification region, which had formed in AISI 8630-IN625 but not in ASTM A182-F22-IN625. These precipitates make the weldment more susceptible to hydrogen embrittlement and provide a low energy fracture path between the discontinuous partially mixed zones.

Influence of tempering temperature on both the microstructural evolution and elemental distribution in AISI 4340 steels

In the present study, the influence of tempering temperature on the microstructural evolution and prior austenite grain boundary segregation of AISI 4340 steels was investigated by transmission electron microscope and atom probe. The transmission electron microscopy results showed a variation in the microstructure and the morphology of carbides with a change in tempering temperature. Additionally, the chemical compositions of the prior austenite grain boundaries and carbides were quantified by atom probe tomography. An increase in the tempering temperature led to a decrease in the amount of carbon segregated at the prior austenite grain boundary from 7.9 to 1.3 at.%. It was found that a higher tempering temperature can accelerate the diffusion of carbon from the prior austenite grain boundary into carbide. However, phosphorus atoms were segregated mainly at the prior austenite grain boundary in steel tempered at 400°C (up to 0.18 at.%). It was found that formation of film-like carbide and phosphorus segregation along the prior austenite grain boundary is the main cause of embrittlement in steel tempered at 400°C.

Metastable precipitate in a duplex martensite

The crystal structure and chemical composition of the strengthening precipitates in an Fe- 11.8 pct Cr-8.5 pct Ni-1.8 pct Ti-3.8 pct Mo martensite + ferrite duplex steel were determined by transmission electron microscopy (TEM). The study revealed that a metastable precipitate phase formed in the ferrite and martensite phases during the initial stages of aging. The meta- stable phase was proposed to have a hexagonal crystal structure similar to that reported for the omega phase in Ti alloys. Prolonged aging formed an equilibrium orthorhombic precipitate phase with a Ni3(Mo, Ti) stoichiometry. The higher dislocation density in martensite accelerated the precipitation reaction, and the transition to the equilibrium precipitate occurred with shorter aging times compared to ferrite. The details of the electron diffraction and analytical electron microscopy studies of the precipitates are described.

Research Progress on Friction Stir Welding of Pipeline Steels

Friction Stir Welding (FSW) has been widely commercialized to join aluminum alloys, but is yet to be broadly applied to structural steels. The primary difficulty in welding steels relates to severe loads and temperatures experienced at the interface between the FSW tool and the base material. These conditions are challenging even for the most advanced and expensive tool materials. However, within the last five years, tool advancements have begun to enable FSW of steels. Polycrystalline boron nitride (PCBN), tungsten-rhenium alloys, and mixtures thereof appear to be capable of producing sound welds in steel. This paper describes the results of a continuing study on the FSW of pipeline steels. Pipe grades from API X65 to X120 were subjected to FSW. Strength and toughness measurements using the crack tip opening displacement test were performed. The weld microstructure was evaluated using optical, scanning electron, and transmission electron microscopy. A computational fluid dynamics model was developed to better understand the effect of process parameters on thermal cycles, strain rates and strain experienced by material in the weld stir zone. The results indicate that the microstructure and properties of the welds have little dependence on the tool material, while significant variations in properties were observed between steels produced by different manufacturers. In general, obtaining high levels of toughness on par with gas metal arc mechanized girth welds appears difficult when using the FSW process. The results emphasize the need for a better understanding on the role of process parameters on microstructural evolution and weld quality during FSW of pipeline steels. As a full-scale demonstration of FSW on pipeline steels, several circumferential girth welds were produced in 762 mm (30 inch) diameter X80 pipe. The results of these efforts are discussed.Copyright