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At least 19 records

In Situ Transmission Electron Microscopy of High-Temperature Inconel-625 Corrosion by Molten Chloride Salts

This paper describes an approach to monitor high temperature molten chloride (MgCl 2 -NaCl-KCl) salt corrosion of Inconel-625 alloy in real time at high spatial resolution. The approach is based on a micro-environmental-cell assembly integrated into a transmission-electron-microscope goniometer to examine in situ the salt-alloy interface during corrosion, employing real time electron diffraction and imaging. It establishes procedures to minimize incorporation of H 2 O or O 2 from atmosphere in the chloride salts during sample fabrication and corrosion, which is critical to understanding the fundamental corrosion mechanisms. A clustering algorithm and a 2D Gaussian fit function are used to determine diffraction spot intensities in in situ diffraction patterns, to quantify alloy corrosion. This facilitates quantitative observation of the evolution of individual grains, in contrast to conventional macroscopic corrosion rate quantification. The isothermal corrosion rate of Inconel-625 in an anhydrous, unoxidized salt-stack is 220 ± 30 μm year -1 at 700 °C and 350 ± 20 μm year -1 at 800 °C. However, the corrosion rate at 700 °C increases five-fold to 1000 ± 170 μm year -1 when the salt stack is air-exposed, indicating the dominant effects of hydrated or oxidized impurities on corrosion acceleration. Furthermore, real time imaging of the microstructure evolution suggests that corrosion is initiated at grain boundaries.

14 SOLAR ENERGY↗

Post-Test Microstructural Analysis of Particle Impact-Tested Wrought Inconel, Additively Manufactured Inconel and Wrought Monel Targets

Particle impact testing in high pressure oxygen was performed to evaluate ignition susceptibility of Inconel 718 and Monel 400. Sapphire particles (1.5-mm diameter) under high pressure oxygen, travelling at hypersonic speeds, made impact with metal targets, resulting in surface indentations. This report details the post-test characterization of impact craters observed on three metallic target samples: wrought nickel-based superalloy Inconel 718 (IN718), additively manufactured Inconel 718 (AM-IN718) and nickel-copper alloy, Monel 400.

Ochoa, Ngozi C.↗

Corrosion of SS 316, Inconel 617, Inconel 625 in molten chloride salt with emphasis on the speciation of Cr, Ni, and Co in molten salt matrix by XAFS

Dr. Hartmann’ report summarizes the corrosion behavior of materials used in the construction and operation of molten salt reactors which is is of great interest to the molten salt reactor (MSR) community. In the present study we intent to decipher the very elemental phenomena on the corrosion of austenitic chromium-containing stainless steel SS316, as well as Inconel 625 and ASME-coded high temperature Alloy (Inconel) 617. We initiated and are in continuation of conducting ampoule type corrosion testing at 550 °C and 650 °C to determine chromium diffusivity and the related activation energy as well as the speciation of the corrosion products.

36 MATERIALS SCIENCE↗

Theory and Apparatus for Measurement of Emissivity for Radiative Cooling of Hypersonic Aircraft with Data for Inconel and Inconel X

The importance of radiation as a means of cooling high-supersonic- and hypersonic-speed aircraft is discussed to show the need for measurements of the total hemispherical emissivity of surfaces. The theory underlying the measurement of the total hemispherical emissivity of surfaces is presented, readily duplicable apparatus for performing the measurements is described, and measurements for stably oxidized Inconel and Inconel X are given for the temperature range from 600 F to 2,000 F.

MATERIALS, PROPERTIES - THERMAL↗

Magnetic susceptibility of Inconel alloys 718, 625, and 600 at cryogenic temperatures

After a hydrogen fuel bleed valve problem on the Discovery Space Shuttle was traced to the strong magnetization of Inconel 718 in the armature of the linear variable differential transformer near liquid hydrogen temperatures, the ac magnetic susceptibility of three samples of Inconel 718 of slightly different compositions, one sample of Inconel 625, and on sample of Inconel 600 were measured as a function of temperature. Inconel 718 alloys are found to exhibit a spin glass state below 16 K. Inconel 600 exhibits three different magnetic phases, the lowest-temperature state (below 6 K) being somewhat similar to that of Inconel 718. The magnetic states of the Inconel alloys and their magnetic susceptibilities appear to be strongly dependent on the exact composition of the alloy.

Goldberg, Ira B.↗

Probing layered structure of Inconel 625 coatings prepared by magnetron sputtering

Coating/substrate interface and oxide layers present in Inconel 625 film may cause significant impacts on its corrosion behavior. However, layered structure of Inconel 625 coatings remains poorly understood due to its requirement of high spatial resolution. Here we have applied X-ray reflectometry (XRR) to probe the layered structure of magnetron-sputtered Inconel 625 film with atomic spatial resolution. Our results indicate that there exists a 2 nm thick Cr-rich Inconel sublayer underneath the principal film. On top of the principal film, it is found a 2 nm thick oxide layer mainly consisting of NiO. In addition, we detected ~2 Å contamination layer on the sapphire substrate, although argon ion sputter cleaning had been applied to the substrate prior to deposition. By comparing the coatings with different deposition time, we observed that the thickness of principal Inconel 625 layer grows linearly with deposition time, with all other layers remaining constant. Our findings provide insight into the layered structures of Inconel 625 coatings with atomic-scale spatial resolution, and provide directions for future efforts that aim to improve the corrosion resistance of Inconel 625 coatings.

14 SOLAR ENERGY↗

Electrochemical, Polarization, and Crevice Corrosion Testing of Inconel X750: A Supplement to the Environmental Control and Life Support System Sustaining Metal Materials Compatibility Study

In previous studies, electrochemical test results were experimentally acquired and then presented for several noble alloys in two specific solutions representative of waste liquids generated or present within the Environmental Control and Life Support System (ECLSS) aboard the International Space Station (ISS). Subsequently, another metal candidate, Inconel X750, has been submitted and was subjected to the same test routines in the same solutions and evaluated with the same statistical/analytical methodologies as those utilized in the earlier studies. Previous studies included three titanium grades, (Commercially Pure, 6Al-4V alloy, and 6Al-4V Low Interstitial alloy), two nickel-chromium alloys (Inconel® 625 and Hastelloy® C276), one high tier stainless steel (Cronidur® 30), and a nickel-titanium alloy (Nitinol 60). Thus far, all candidate alloys have exhibited excellent corrosion protection and galvanic compatibility attributes and have been deemed qualified materials for application within the ECLSS facility. Inconel X750 now joins that group. The titanium alloys gave the best results of all the metal candidates by demonstrating superior nobility and galvanic protection properties. It is worth noting that the corrosion performance properties for the three titanium alloys were essentially indistinguishable. As such and for expediency, this study and all future evaluations will refer only to the comparative properties already documented for Titanium 6Al-4V as this alloy is representative of all three alloys and considered to be more mainstream. Now the measured corrosion properties for Inconel X750 were very similar to those determined previously for Inconel 625 and Hastelloy C276 which were also determined to be very high performers. For the current effort, the results have clearly shown that Inconel X750 possesses exceptional anti-corrosion attributes comparable to metals in the highest tier of the galvanic series. Overall, one can conclude that Inconel X750 is quite noble, highly corrosion resistant and galvanically compatible with the other metal groups from both an electrochemical perspective and a long-term exposure scenario. This was clearly demonstrated after utilizing the same techniques as those applied in previous studies which included linear, Tafel and cyclic polarization, galvanic coupling with each of the other metal candidates, and pitting/crevicing assessments after one full year of immersion in the subject test solutions. Attributes defining the nobility and anti-corrosion capabilities for X750 appear to be on par with all the other candidates thus far and this alloy can now be classified as ‘excellent’ exhibiting very high resistance toward general, localized, and galvanic corrosion in the subject test media.

Lee, R. E.↗

Radiation-Induced Defect Formation Kinetics in Inconel–Cu Multimetallic Layered Composites

This study investigates the stability of Inconel–Cu Multimetallic Layered Composites (MMLCs) in nuclear reactor applications using Molecular Dynamics simulations. The focus is on understanding the underlying mechanisms governing the properties of MMLCs for advanced nuclear reactors, specifically, the mechanochemistry of the interface between Inconel and copper alloys. The selection of Inconel–Cu MMLCs is primarily due to copper’s superior thermal conductivity, enhancing heat management within reactors by preventing hotspots and ensuring uniform temperature distribution. This research examines Incoloy 800H and two Inconel variants (718 and 625), assessing their stability at 1000 K after exposure to 10 keV collision cascades up to 0.12 dpa. Notable findings include defect clustering on the {1 2 0} family of planes of Inconel and Cu, with Stacking Faults and Lomer–Cottrell locks on the Inconel side.

Ramesh, Rajesh↗

Strength Differential Measured in Inconel 718: Effects of Hydrostatic Pressure Studied

Aeropropulsion components, such as disks, blades, and shafts, are commonly subjected to multiaxial stress states at elevated temperatures. Experimental results from loadings as complex as those experienced in service are needed to help guide the development of accurate viscoplastic, multiaxial deformation models that can be used to improve the design of these components. During a recent study on multiaxial deformation (ref. 1) on a common aerospace material, Inconel 718, it was shown that the material in the aged state exhibits a strength differential effect (SDE), whereby the uniaxial compressive yield and subsequent flow behavior are significantly higher than those in uniaxial tension. Thus, this material cannot be described by a standard von Mises yield formulation. There have been other formulations postulated (ref. 2) that involve other combinations of the stress invariants, including the effect of hydrostatic stress. The question remained as to which invariants are necessary in the flow model. To capture the physical mechanisms occurring during deformation and reflect them in the plasticity formulation, researchers examined the flow of Inconel 718 under various amounts of hydrostatic stress to determine whether or not hydrostatic stress is needed in the formulation. Under NASA Grant NCC3-464, monitored by the NASA Glenn Research Center, a series of tensile tests were conducted at Case Western Reserve University on aged (precipitation hardened) Inconel 718 at 650 C and with superimposed hydrostatic pressure. Dogbone shaped tensile specimens (3-mm-diameter gauge by 16-mm gauge length) and cylindrical compression specimens (3-mm-diameter gauge by 6-mm gauge length) were strain gauged and loaded in a high-pressure testing apparatus. Hydrostatic pressures were obtained with argon and ranged from 210 to 630 MPa. The aged Inconel 718 showed a pronounced difference in the tension and compression yield strength (i.e., an SDE), as previously observed. Also, there were no significant effects of hydrostatic pressure on either the tensile and compressive yield strength (see the graph) or on the magnitude of the SDE. This behavior is not consistent with the pressure-dependent theory of the SDE, which postulates that the SDE is associated with pressure-dependent and/or internal friction dependent deformation associated with non-Schmid effects at the crystal level (refs. 3 and 4). Flow in Inconel 718 appears to be independent of hydrostatic pressure, suggesting that this invariant may be removed from the phenomenological constitutive model. As part of an ongoing effort to develop advanced constitutive models, Glenn s Life Prediction Branch coordinated this work with that of research on the multiaxial deformation behavior of Inconel 718 being conducted at Pennsylvania State University under NASA Grant NCC597.

Lewandowski, John J.↗

Characterization of Properties of Laser Powder Bed Fusion 3D-Printed Inconel 718 for Centrifugal Turbomachinery Applications

Here, this paper presents the results of a comprehensive effort to characterize the properties of Inconel 718 produced by a form of laser powder bed fusion (LPBF) additive manufacturing (AM) or 3D-printing, subsequently subjected to hot isostatic pressing (HIP) and heat treatment according to standards F3055-14a and AMS 5663, respectively. Material property data, while broadly available for traditional Inconel 718 presentations (e.g. forgings or castings), is currently lacking for the 3D-printed material. It is expected that while limited in size, the experimental data sets presented provide sufficient information to glean the capability of LPBF Inconel 718. These include: 1) Chemical composition, electron backscatter diffraction (EBSD), and x-ray energy dispersive spectroscopy (XEDS) characterization of 3D-printed material structure; 2) Tensile properties — 0.2% yield stress, ultimate stress, modulus of elasticity, and elongation to failure — based on 108 samples, as functions of temperature and sample print orientation; 3) Creep rupture data including the Larson-Miller parameter, based on 21 samples; and 4) High cycle fatigue data based on 21 samples as a function of temperature. Results are compared to available standards and/or data for forged, cast, and other AM Inconel 718. A key observation of this study, based on the EBSD results, is that while the material appears to approach full recrystallization following heat treatment, there is a detectable fraction of the material that does not fully recrystallize, resulting in a material with mechanical properties (e.g. yield stress, creep rupture) measurably lower than those of forgings, but higher than those of castings.

30 DIRECT ENERGY CONVERSION↗

Grain size effect on corrosion behavior of Inconel 625 film against molten MgCl 2 -NaCl-KCl salt

This study evaluated the grain size effect of Inconel 625 film against molten chloride salt. It is found that larger grain size Inconel 625 exhibits better corrosion resistance by reducing Cr depletion. ~ 2 nm surface NiO layer of Inconel 625 is incapable of compensating the negative effects from more initiation corrosion sites. Mo is the least likely leached element and its enrichment occurs in Cr-depleted regions as a result of Mo diffusion. Mg and Cl are two most seen salt elements in all corroded samples, while K and Na only attack Inconel 625 with the smallest grain size.

14 SOLAR ENERGY↗

Report on Evolution of Inconel 718 Following HFIR Irradiation

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 after irradiation in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) to assess its potential use as a structural material. The structural components near the outlets of several proposed reactor cores will experience significant neutron fluxes and outlet coolant temperatures ranging from the hot standby temperature of 300 °C to nearly 550 °C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. In FY21, three heat treatments were designed and conducted to simplify the microstructure and to determine how each precipitating phase contributed to the overall strength. In FY21, baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600 °C to serve a comparison to the irradiated properties. Four capsules containing 3D printed Inconel 718 were inserted into HFIR in FY21 for a matrix of two temperatures and two doses. The lower of the two doses was available for characterization in FY22. Multiple heat treatments of Inconel 718 irradiated to nominal conditions of 2 displacements per atom (dpa) at either 300 or 600 °C were strained with uniaxial tensile tests at the Irradiated Material Examination and Testing (IMET) Facility to discern the mechanical properties. Transmission electron microscopy was performed to correlate the observed mechanical properties with nanoscale features. The initially homogenous AM718-HM increased in strength at both irradiation temperatures based on a high density of nanometer-scale radiation-induced cavities at lower temperature and nucleation and growth of γ" precipitates at higher temperatures. The precipitate-hardened AM718-HT2 showed very small differences in strength before and after irradiation: the contribution to strength from γ" precipitates was replaced with dislocation loops. Because the radioactivity of the nickel superalloys from neutron activation limited the scope of the analysis, a feasibility study examined the possibility of an ultra-miniature specimen geometry, colloquially SS-Tiny (SS-T), for mechanical property determination using the nonirradiated Inconel 718. This study found an overestimation of ductility from the SS-T geometry with yield strength and ultimate tensile strength slightly above the SS-J2 geometry: this could be contributed to a reduction in specimen thickness.

36 MATERIALS SCIENCE↗

Solid-State Transformation of an Additive Manufactured Inconel 625 Alloy at 700 °C

Inconel 625, a nickel-based superalloy, has drawn much attention in the emerging field of additive manufacturing (AM) because of its excellent weldability and resistance to hot cracking. The extreme processing condition of AM often introduces enormous residual stress (hundreds of MPa to GPa) in the as-fabricated parts, which requires stress-relief heat treatment to remove or reduce the internal stresses. Typical residual stress heat treatment for AM Inconel 625, conducted at 800 °C or 870 °C, introduces a substantial precipitation of the δ phase, a deleterious intermetallic phase. In this work, we used synchrotron-based in situ scattering and diffraction methods and ex situ electron microscopy to investigate the solid-state transformation of an AM Inconel 625 at 700 °C. Our results show that while the δ phase still precipitates from the matrix at this temperature, its precipitation rate and size at a given time are both smaller when compared with their counterparts during typical heat treatment temperatures of 800 °C and 870 °C. A comparison with thermodynamic modeling predictions elucidates these experimental findings. Our work provides the rigorous microstructural kinetics data required to explore the feasibility of a promising lower-temperature stress-relief heat treatment for AM Inconel 625. The combined methodology is readily extendable to investigate the solid-state transformation of other AM alloys.

36 MATERIALS SCIENCE↗

Spectral Emittance of Uncoated and Ceramic-Coated Inconel and Type 321 Stainless Steel

The normal spectral emittance of Inconel and type 321 stainless steel with different surface treatments was measured at temperatures of 900, 1,200, 1,500, and 1,800 F over a wavelength range of 1.5 to 15 microns. The measurements involved comparison of the radiant energy emitted by the heated specimen with that emitted by a comparison standard at the same temperature by means of a recording double-beam infrared spectrophotometer. The silicon carbide comparison standard had previously been calibrated against a laboratory black-body furnace. Surface treatments included electropolishing, sandblasting, electro-polishing followed by oxidation in air for 1/2 hour at 1,800 F, sandblasting followed by oxidation in air for 1/2 hour at 1,800 F, application of National Bureau of Standards coating A-418, and application of NBS ceramic coating N-143. The normal spectral emittance of both alloys in the electropolished condition was low and decreased very slightly with increasing wavelength while in the sandblasted condition it was somewhat higher and did not vary appreciably with wavelength. The oxidation treatment greatly increased the normal spectral emittance of both the electropolished and sandblasted type 321 stainless steel specimens and of the electropolished Inconel specimens and introduced some spectral selectivity into the curves. The oxidation increased the normal spectral emittance of the sandblasted Inconel specimens only moderately. Of the specimens to which a coating about 0.002 inch thick was applied, those coated with A-418 had higher emittance at all wavelengths than did those coated with N-143, and the coated specimens of Inconel had higher spectral emittance at all wavelengths than did the corresponding specimens of type 321 stainless steel. Both coatings were found to be partially transparent to the emitted energy at this thickness but essentially opaque at a thickness of 0.005 inch. Coated specimens with 0.005 inch or more of coating did not show the effect of the underlying metal on spectral emittance, and there was no significant difference at wavelengths greater than about five microns in the normal spectral emittance of specimens having the two coatings. At shorter wavelengths the normal spectral emittance of specimens coated with A-418 was greater than that of specimens coated with N-143.

Richmond, Joseph C.↗

Tensile Properties and Microstructure of Inconel 718 Fabricated with Electron Beam Freeform Fabrication (EBF(sup 3))

Electron beam freeform fabrication (EBF3) direct metal deposition processing was used to fabricate two Inconel 718 single-bead-width wall builds and one multiple-bead-width block build. Specimens were machined to evaluate microstructure and room temperature tensile properties. The tensile strength and yield strength of the as-deposited material from the wall and block builds were greater than those for conventional Inconel 718 castings but were less than those for conventional cold-rolled sheet. Ductility levels for the EBF3 material were similar to those for conventionally-processed sheet and castings. An unexpected result was that the modulus of the EBF3-deposited Inconel 718 was significantly lower than that of the conventional material. This low modulus may be associated with a preferred crystallographic orientation resultant from the deposition and rapid solidification process. A heat treatment with a high solution treatment temperature resulted in a recrystallized microstructure and an increased modulus. However, the modulus was not increased to the level that is expected for Inconel 718.

Bird, R. Keith↗

A Discrete Dendrite Dynamics Model for Epitaxial Columnar Grain Growth in Metal Additive Manufacturing with Application to Inconel

Epitaxial columnar grain growth is a prevalent microstructural feature in the additive manufacturing (AM) of metal components such as Inconel, with cubic unit cell crystal lattice structure (face centered cubic (FCC) or body centered cubic (BCC)). These columnar grains evolve from the partly molten grains in the substrate or the solidified metal. This work proposes an efficient model to simulate the competitive growth of epitaxial columnar dendritic grains. The proposed model tracks the dynamic changes in the dendrites emanating from discrete points along the solid/liquid interface of a quasi-steady melt pool (MP). These dynamic changes include convergence and divergence of growing dendrites. The model is extended to predict the microstructure of large 3D parts and experimentally validated by comparing the simulation results for laser powder bed fusion (L-PBF) and wire-arc additive manufacturing (WAAM) processes. The microstructure and pole figures are predicted for Inconel 718 samples produced by L-PBF and Inconel 740H samples produced by WAAM processes. Finally, the model predictions compare well with the observed microstructure and pole figures results for both the L-PBF and WAAM processes.

20 FOSSIL-FUELED POWER PLANTS↗

Helium tribology of Inconel 617 subjected to laser peening for high temperature nuclear reactor applications

Inconel 617 is among the best candidates for utilization in high temperature gas cooled reactor tribo-components. However, the combined effects of sliding contact, along with intermittent idle times and very high temperature material degradation, deteriorates the alloy tribological performance, especially under a helium atmosphere. Laser peening is a surface treatment technique which can enhance the properties at the surface and subsurface by generating deep residual stresses and enhanced microstructure. In this work, we report the tribological behavior of regular laser peened as well as thermally-engineered laser peened Inconel 617 under helium and air atmospheres at 800 °C. In addition to friction and wear studies, the specimens are characterized by different analytical techniques to further understand the mechanisms involved in the peening process and sliding contact. Regardless of the peening process and post-process treatment types, it is observed that laser peening improves the tribological characteristics of Inconel 617. Interestingly, laser peening followed by helium thermal aging shows highly enhanced tribological behavior. This is attributed to the strengthening effect of the laser peening on the surface oxides providing an excellent and lasting protective and lubricating film under helium exposure.

42 ENGINEERING↗