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NASA NTRS2010

Launch Pad Coatings for Smart Corrosion Control

Corrosion is the degradation of a material as a result of its interaction with the environment. The environment at the KSC launch pads has been documented by ASM International (formerly American Society for Metals) as the most corrosive in the US. The 70 tons of highly corrosive hydrochloric acid that are generated by the solid rocket boosters during a launch exacerbate the corrosiveness of the environment at the pads. Numerous failures at the pads are caused by the pitting of stainless steels, rebar corrosion, and the degradation of concrete. Corrosion control of launch pad structures relies on the use of coatings selected from the qualified products list (QPL) of the NASA Standard 5008A for Protective Coating of Carbon Steel, Stainless Steel, and Aluminum on Launch Structures, Facilities, and Ground Support Equipment. This standard was developed to establish uniform engineering practices and methods and to ensure the inclusion of essential criteria in the coating of ground support equipment (GSE) and facilities used by or for NASA. This standard is applicable to GSE and facilities that support space vehicle or payload programs or projects and to critical facilities at all NASA locations worldwide. Environmental regulation changes have dramatically reduced the production, handling, use, and availability of conventional protective coatings for application to KSC launch structures and ground support equipment. Current attrition rate of qualified KSC coatings will drastically limit the number of commercial off the shelf (COTS) products available for the Constellation Program (CxP) ground operations (GO). CxP GO identified corrosion detection and control technologies as a critical, initial capability technology need for ground processing of Ares I and Ares V to meet Constellation Architecture Requirements Document (CARD) CxP 70000 operability requirements for reduced ground processing complexity, streamlined integrated testing, and operations phase affordability. Researchers at NASA's Corrosion Technology Laboratory at KSC are developing a smart, environmentally friendly coating system for early corrosion detection, inhibition, and self healing of mechanical damage without external intervention. This smart coating will detect and respond actively to corrosion and mechanical damage such as abrasion and scratches, in a functional and predictable manner, and will be capable of adapting its properties dynamically. This coating is being developed using corrosion sensitive microcapsules that deliver the contents of their core (corrosion inhibiting compounds, corrosion indicators, and self healing agents) on demand when corrosion or mechanical damage to the coating occurs.

Calle, Luz M.↗

DOE OSTI2024

Discerning the effect of various irradiation modes on the corrosion of Zircaloy-4

Using proton irradiation, this study investigates the individual influence of several factors on the corrosion kinetics of Zircaloy-4 in a hydrogenated water environment simulating a Pressurized Water Reactor (PWR). Using both simultaneous irradiation-corrosion and autoclave corrosion, we separately examine: (i) the effect of pre-irradiation on modifying the structure of the material, (ii) the impact of irradiation on creating defects in the growing oxide layer during corrosion, and (iii) the influence of irradiation on increasing the corrosion potential through radiolysis during corrosion. To replicate neutron-irradiated microstructure, two proton pre-irradiation schedules were employed: Schedule 1 (isothermal irradiation at 350 °C to 5 dpa) to simulate high-temperature PWR conditions, and Schedule 2 (two-step process: irradiation to 2.5 dpa at -10 °C followed by 2.5 dpa at 350 °C) to simulate lower temperature PWR and Boiling Water Reactor (BWR) conditions. Long-term autoclave corrosion testing over 360 days at 320 °C revealed no significant difference between unirradiated samples and those pre-irradiated according to either schedule, with all samples exhibiting sub-cubic kinetics within the pre-transition regime. Irradiated samples underwent Simultaneous Irradiation Corrosion (SIC) tests, corroding in 320 °C water while being irradiated with protons. Corrosion was found to accelerate in all SIC-tested samples relative to autoclave conditions, with the greatest increase observed in non-pre-irradiated samples. Pre-irradiation with either schedule resulted in a slower corrosion rate compared to non-pre-irradiated regions under SIC conditions. The degree of radiolysis observed in the SIC tests surpassed typical PWR conditions, approaching levels found in BWRs. Radiolysis products were identified as the primary contributors to accelerated corrosion, corroborated by radiolysis bar tests. Furthermore, these findings underscore the intricate interactions between irradiation, corrosion, and water chemistry in determining Zircaloy-4 corrosion kinetics within nuclear reactor environments.

Pressurized Water Reactor↗

DOE OSTI2020

Progress in Understanding the Origins of Excellent Corrosion Resistance in Metallic Alloys: From Binary Polycrystalline Alloys to Metallic Glasses and High Entropy Alloys

Some of the factors responsible for good corrosion resistance of select polycrystalline and emerging alloys in chloride solutions are discussed with a goal of providing some perspectives on the current status and future directions. Traditional metallic glass alloys, single phase high entropy alloys (HEAs), early metallic glasses, and high entropy metallic glasses are all emerging corrosion-resistant alloys (CRAs) that utilize traditional strategies for improved corrosion resistance as well as take advantage of some other novel beneficial attributes. These materials enjoy many degrees of freedom as far as choice of both composition and structure, providing great flexibility in the pursuit of superior corrosion resistance. The new materials depart from classical solvent-solute type polycrystalline binary or ternary alloys. Thus, such emerging materials provide significant opportunities to achieve even greater improvements in corrosion resistance in harsh environments. Several examples of the unique corrosion properties of selected materials in the context of modern theories of corrosion are discussed herein. Discussion is restricted to solid-solution binary or ternary polycrystalline alloys, several metallic glass alloys, and single phase HEAs. A common feature of many CRAs is that composition and microstructure often affect both passivity and resistance to localized corrosion that can be divided into initiation, stabilization, and propagation stages. Enormous complexities in protective oxide structures and chemistries and the large number of combinatorial possibilities in newer materials such as HEAs preclude trial-and-error approaches and perhaps even combinatorial experimental design. Computational materials methodologies will be required in the search for new corrosion-resistant alloys in these material classes. The search must consider the best scientific insights available regarding how major and minor alloy additions, as well as various microstructural attributes, contribute to corrosion mitigation. Additional scientific insights, as they emerge, will enable choices beyond the reliance on high concentrations of alloying elements that are known to affect passivity breakdown and pit stabilization. A challenge is to connect the “basic attributes” of an alloy with its properties. The strength of this connection will likely require new scientific principles enabling deep multiphysics insights in order to link feature(s) such as composition and metallurgical phases to the desired corrosion properties. Application of data informatics will likely also play a role given the plethora of variables that are important in corrosion and the difficulty in assessing all relationships. Here, the opportunity exists to accelerate the design of emerging materials for high corrosion resistance.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Fe Coated Optical Fiber for Distributed Corrosion Monitoring in Soil and Aqueous Environment

Natural gas pipeline corrosion represents a substantial cost and safety concern during normal operations. Effective monitoring of corrosion is important to detect and mitigate pipeline risks before corrosion-related catastrophic events happen. Here, we describe the use of Fe-coated optical fiber sensors (OFS) for distributed corrosion monitoring where Fe acts as a corrosion proxy. By using an optical backscatterring reflectometer (OBR), corrosion was monitored based on the increase in backscattered intensity amplitude of the light being passed as Fe undergoes corrosion. The Fe-coated OFSs were prepared with a film thickness between 25-225 nm by an electroless plating approach and corroded by a CO2-saturated acidic electrolyte. The corrosion rate was approximately 2.5 mm/yr for Fe with a film thickness of 30 nm and increased with film thickness. Backscattering-based corrosion rates were supported by visible light transmission measurements, which have been previously demonstrated. Additionally, a correlation between the intermittent transmission and residual Fe film thickness during corrosion of Fe was established. Corrosion was measurable out to > 100 m which is a significant improvement over our previous work showing corrosion sensing at < 10 m. The corrosion sensor was also tested in soil at >1 ft depth. Fe-coated OFS was loaded into a Draka cable which provides mechanical support during fiber deployment and installation into either acidified soil, top-soil, or sandy soil.

aqueous environment↗

DOE OSTI2022

In Situ High-Temperature TEM Observation of Inconel Corrosion by Molten Chloride Salts with N 2 , O 2 , or H 2 O

Here, in situ transmission electron microscopy (TEM) diffraction and imaging techniques are used to monitor and quantify corrosion of Inconel-625 by pure molten chloride salts (MgCl 2 – NaCl – KCl) at 500 °C–800 °C in 1.0 atm inert N 2 or pure O2, or by salts which are controllably hydrated in a high vacuum chamber. The isothermal corrosion rate R in inert N 2 increases from 203 ± 30 μ m year –1 at 700 °C to 463 ± 30 μ m year –1 at 800 °C. An oxygen ambient causes a six-fold increase to R = 1261 ± 170 μ m year –1 at 700 °C. Salt hydration dramatically accelerates corrosion to R > 3 × 10 5 μ m year –1 at 700 °C while it leads to a more moderate R = 95 ± 20 and 486 ± 30 μ m year –1 at 500 °C and 600 °C, respectively. These isothermal corrosion rates indicate that the molten chloride corrosion is significantly accelerated by salt hydration at temperatures above 600 °C, where corrosion is aggravated by increased generation and solubility of corrosive HCl gases. Hence, to reduce rate of corrosion it is important to both avoid incorporation of H 2 O into the system at each stage and ensure proper flushing of the system before increasing the temperature beyond 600 °C. Compositional analysis of the corroded cells indicate that corrosion in O 2 ambient is dominated by oxidation of metals by O 2 gas dissolved in the chloride melt, but corrosion in H 2 O ambients is caused by chlorination of metals by dissolved HCl gas and MgOH + ions. So, to reduce rate of corrosion, steps should be taken to tailor chloride melt compositions that has low solubility for HCl and O 2 . All of our corroded samples exhibit passive-protective oxide layers of Cr, Mg, and Ni. In addition, distinct volatile compounds of Ni, Mo and Cr involving NiCl 2 , (Na,K) 2 MoO 4 and CrO 2 (OH) 2 are detected in N 2 , H 2 O, and O 2 ambients, respectively. We believe that corrosion acceleration can be minimized by minimizing formation of volatile by-products or promoting reactions that could convert these volatile compounds to solid phases, as these volatile compounds led to destruction of protective oxide layers.

14 SOLAR ENERGY↗

DOE OSTI2020

Modelling uranium dioxide corrosion under repository conditions: A pore-scale study of the chemical and thermal processes

This paper investigates the corrosion behaviors of spent uranium dioxide (UO 2 ) fuel when placed in geological repositories. We performed pore-scale reactive transport simulations of the UO 2 corrosion process in a defective fuel rod with different orientations of breach or fracture on its clad. It is found that the corrosion rate has strong dependency on the breach orientation. The highest corrosion rate of UO 2 is calculated when the angle between the groundwater flow direction and the clad fracture reaches 180°. UO 2 corrosion simulations with different flow rates are compared. The results show the higher flow rate accelerates the corrosion of UO 2 fuel. The effect of pH on the corrosion process is also determined. It is indicated that higher pH can limit the corrosion of UO 2 by reducing the reaction rate. The dependence of reaction rate and time on reactive surface area is explored. Spent fuel with lower surface area demonstrates longer lifetime under corrosion conditions. A numerical model coupling thermal conduction and chemical reactions is developed to assess the impact of temperature on the process of UO 2 corrosion. The results show that higher temperature leads to larger corrosion rates for UO 2 . Here, the predicted reaction rates are higher in comparison with the isothermal results. Hence, our results can help improve the fundamental understanding of UO 2 corrosion in geological repositories for long-term storage of spent nuclear fuels and provide guidance for the safe operations and selection of appropriate repositories.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Fe-Coated Optical Fiber for Distributed Corrosion Monitoring in Soil and Aqueous Environments

Natural gas pipeline corrosion represents a substantial cost and safety concern during normal operations. The effective and real-time monitoring of corrosion is important to detect and mitigate pipeline risks before corrosion-related catastrophic events happen. Here, we describe the use of iron (Fe) coated optical fiber sensors (OFS) for distributed corrosion monitoring where Fe acts as a corrosion proxy. By using an optical backscattering reflectometer (OBR), corrosion was monitored based on the increase in the backscattered intensity amplitude of the light being passed as Fe underwent corrosion. The Fe-coated OFSs were prepared with a film thickness between 25–225 nanometers (nm) by an electroless plating approach and corroded by a carbon dioxide (CO2)-saturated acidic electrolyte. The corrosion rate (CR) was approximately 2.5 millimeters (mm)/year for Fe with a film thickness of 30 nm and increased with film thickness. Backscattering-based CRs were supported by visible light transmission measurements, which have been previously demonstrated. Additionally, a correlation between the intermittent transmission and residual Fe film thickness during the corrosion of Fe was established. The corrosion was measurable out to > 100 meters (m), which is a significant improvement over our previous work, which showed corrosion sensing at < 10 m. The corrosion sensor was also tested in soil at > 1 foot depth.

corrosion↗

DOE OSTI2025

Corrosion Testing of Refractory inContact with Molten Glasses Designed for Waste Vitrification - VSL Touchpoint Matrix Glasses

It is known that the predictive life of the refractory ceramic liner of nuclear waste glass melters is conservative, as demonstrated by performance of these materials such as in the Defense Waste Processing Facility (DWPF). The motivation for this task is to maximize the useful life of the melters that will be operated at the Waste Treatment and Immobilization Plant (WTP), which will in turn minimize procurement and disposal costs and melter outage times, as well as to identify maximum loadings in the waste glass of those species that corrode melter components. This task was initiated jointly with Pacific Northwest National Laboratory (PNNL) with the objective to develop a methodology and model to enable more accurate prediction of refractory service life under prototypic conditions from laboratory-scale material corrosion tests. Refractory corrosion is generally reported as physical material loss, measured in units of distance (e.g., inch) or as physical material loss rate, measured in units of distance per time (e.g., inch/day). In post-operational melters, the refractory corrosion is measured directly, sometimes reported as corrosion depth. Crucible tests are used in the laboratory to accelerate the refractory corrosion to facilitate a meaningful measurement in a commensurate amount of time. Crucible tests are particularly useful in understanding refractory corrosion across a large glass composition space, where operational testing would be prohibitive. Some of the critical parameters that are known to influence refractory corrosion by molten glass in a crucible test are temperature, system redox, molten salt phases, glass chemistry, and test duration. The majority of data collected for Monofrax® K-3 (hereafter referred to as K-3) corrosion is from crucible tests, but a small amount comes directly from scaled and production melters. Crucible test data has been collected under varying conditions, whereas data collected from operational melters is relatively fewer and represents conditions specific to the melter campaign. The result is that the published data can be grouped and analyzed in multiple ways, not all of which are readily comparable. The Standard Test Method for Isothermal Corrosion Resistance of Refractories to Molten Glass (ASTM C621) outlines the general guidelines used across industry. That method describes a sealed, static test in which the surface area of the refractory coupon and the volume of glass are fixed. A significant portion of the crucible data pertaining to nuclear waste glasses has been collected in a modified configuration; the most notable differences being the surface area of the refractory coupon to volume of the glass and use of a method for bubbling the melt. To our knowledge, the influence of those parameters on the refractory corrosion has not been quantified. In this work, it was determined that static tests and bubbled tests would be performed. Savannah River National Laboratory (SRNL) was tasked with setting up and performing static testing while PNNL was tasked with setting up and performing bubbled testing. Initial activities were performed to establish laboratory methods that reproduce data comparable to existing data sets of K-3 refractory corrosion by low activity waste (LAW) and high-level waste (HLW) glass compositions. Later activities were focused on refining the test parameters to establish a standard test practice to be used between Laboratories and collecting additional data to be used in the enhanced waste glass model development. This document serves primarily to convey the refractory loss measurement results from corrosion testing of K-3 refractory with waste glass compositions developed for use in the WTP melters. The data will be used in the enhanced property/composition models being developed for waste glass vitrification and melter operations.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Development of Corrosion Resistant Coatings for Structural Materials for Liquid Fueled Molten Salts Reactors Applications (Final Report)

Current structural alloys, code certified for the MSRs temperature ranges, contain high levels of chromium, making them highly susceptible to molten halide salt corrosion. One potential solution to circumvent the need for code certification of novel alloys, which is expensive and time consuming, is to design claddings that will protect the underlying code certified materials from corrosion damage during operation. In this work, we examined the corrosion of Ni and Cu electroplated, Ni and CuNi weld overlay, Mo-laser clad, and carburized claddings on SS316H for use in molten salt reactor environments. After characterization of the cladded materials (Task 1), static corrosion tests were used to assess corrosion resistance of the claddings in typical molten fluoride salts (Task 2). The corrosion tests were performed in molten FLiNaK at 700°C up to 1000 hours. Pre- and post-corrosion Scanning Electron Microscopy (SEM), energy-dispersive-spectroscopy (EDS), Transmission Electron Microscopy (TEM), X-ray Diffraction (XRD) and glow-discharge-optical-emission-spectroscopy (GDOES) were performed on cladding cross-sections and surfaces to evaluate degradation. The Cu and Ni electroplated samples, as well as the carburized samples, showed excellent corrosion resistance relative to the bare SS316H. To assess high temperature cladding stability, ageing experiments were performed at temperatures up to 900 C in inert atmosphere for the electroplated and carburized samples and a diffusion model was developed to predict long term cladding behavior (Task 3). It was found that the Cu cladding was basically insensitive to the high temperature ageing, except for small secondary phases forming at the interface. On the other hand, the Ni electroplated cladding experienced significant interdiffusion. Nevertheless, the gain in corrosion resistance for a 100μm Ni electroplated cladding is phenomenal, with more than 50% reduction in chromium dissolution from the substrate material for the first 15 years of salt exposure at 700°C. To assess radiation resistance and phase stability, high-temperature 4MeV Ni heavy ion irradiation was performed across the cladding/substrate interface up to 50 displacement-per-atom (DPA) at 500°C and 700°C to assess the phase stability and irradiation behaviors of the electroplated systems (Task 4). The Ni and Cu electroplated systems did not experience void swelling at the contrary to the SS316H substrate due to their nanocrystalline nature. Some level of recrystallization was observed in the cladding, as well as radiation induced segregation and enhanced diffusion. The interface acted as a potent sink for point defects with the presence of a void denuded zone. The mechanical properties of the claddings were assessed using thermal shock, micro-indentation, nano-indentation, and four-point bend testing experiments (Task 5). These experiments were performed on the claddings in as-received, corroded, irradiated, and thermally aged states to determine the effects of typical molten salt reactor environments on cladding integrity. No significant mass loss was observed after repeated thermal shocks. While the electroplated samples softened after high-temperature ageing, irradiation hardening compensate this effect, such that there is little different with the as-received materials. The results of these experiments suggest that the electroplated (copper/nickel) show the greatest promise for application in molten salt reactor development. These claddings prevented any chromium dissolution from occurring during the static corrosion experiments. Additionally, they demonstrated favorable properties for high temperature diffusion, phase stability, interfacial mechanical properties, and irradiation resistance. Weld-overlay cladding are also of great interest and could reach properties similar to the electroplated samples upon optimization (especially with multiple weld passes). The carburized SS316H showed excellent behavior as well, but more work needs to be done to assess their long-term stability. Finally, the Mo-laser clad system was not pursued further due to the manufacturing challenges. It is also worth noting that the Ni cladding systems should behave relatively well in terms of weldability since the Ni-weld overlay microstructure and associated corrosion rate are sound. While the NiCu weld-overlay has even lower corrosion rates than the Ni-weld overlay, more studies on welding of Cu-electroplated systems are necessary since Cu clusters are known to embrittle steels.

36 MATERIALS SCIENCE↗

NASA NTRS2002

Detection of Intergranular Corrosion in Cold Plate Face Sheets

Cold plates are critical for cooling electronic systems in the shuttle. As a result of the environmental conditions in which they operate, water can condense between them and a support shelf. In some cases, this water results in intergranular corrosion in the face sheet. If the intergranular corrosion sufficiently penetrates the face sheet, a coolant leak could occur and jeopardize cold plate operation. This paper examines techniques for detecting and characterizing the intergranular corrosion, to enable recertification of cold plates that have been in operation for 15 plus years. Intergranular corrosion was artificially induced in the face sheets of a series of cold plate specimens using an electrochemical process. Some of the cold plate specimens were separated for destructive characterization of the extent of corrosion produced by the electrochemical process and to insure the induced corrosion was intergranular. The rest of the specimens were characterized nondestructively using several techniques. X-ray tomography and ultrasonic techniques provided the best indication of corrosion in these specimens and will be the focus of this paper. An x-ray tomography technique was shown to be the most effective technique for characterizing depth of the intergranular corrosion. From these measurements, corrosion profile maps were developed that were consistent with subsequent destructive evaluations of the specimens. This enabled the assessment of NDE (ondestructive evaluation) standards to evaluate the viability of other NDE techniques. Due to system constraints, a different technique must be used to inspect an entire cold plate. An ultrasonic technique was shown to be very reliable for detection of corrosion in the unbacked regions of the face sheet. The ultrasonic technique was performed in an alcohol bath to avoid additional corrosion during the NDE evaluation. A pulse echo technique that focuses on the RMS value of the signal is shown to be very sensitive to the presence of intergranular corrosion.

Winfree, William P.↗

NASA NTRS2010

A Multifunctional Coating for Autonomous Corrosion Control

Corrosion is a destructive process that often causes failure in metallic components and structures. Protective coatings are the most commonly used method of corrosion control. However, progressively stricter environmental regulations have resulted in the ban of many commercially available corrosion protective coatings due to the harmful effects of their solvents or corrosion inhibitors. This work concerns the development of a multifunctional, smart coating for the autonomous control of corrosion. This coating is being developed to have the inherent ability to detect the chemical changes associated with the onset of corrosion and respond autonomously to control it. The multi-functionality of the coating is based on microencapsulation technology specifically designed for corrosion control applications. This design has, in addition to all the advantages of other existing microcapsules designs, the corrosion controlled release function that allows the delivery of corrosion indicators and inhibitors on demand only when and where they are needed. Corrosion indicators as well as corrosion inhibitors have been incorporated into the microcapsules, blended into several paint systems, and tested for corrosion detection and protection efficacy.

Calle, Luz M.↗

NASA NTRS2012

A Multifunctional Smart Coating for Autonomous Corrosion Control

Corrosion is a destructive process that often causes failure in metallic components and structures. Protective coatings are the most commonly used method of corrosion control. However, progressively stricter environmental regulations have resulted in the ban of many commercially available corrosion protective coatings due to the harmful effects of their solvents or corrosion inhibitors. This work concerns the development of a multifunctional, smart coating for the autonomous control of corrosion. This coating is being developed to have the inherent ability to detect the chemical changes associated with the onset of corrosion and respond autonomously to control it. The multi-functionality of the coating is based on micro-encapsulation technology specifically designed for corrosion control applications. This design has, in addition to all the advantages of other existing microcapsules designs, the corrosion controlled release function that allows the delivery of corrosion indicators and inhibitors on demand only when and where needed. Corrosion indicators as well as corrosion inhibitors have been incorporated into microcapsules, blended into several paint systems, and tested for corrosion detection and protection efficacy. This

Calle, Luz Marina↗

DOE OSTI2025

Fe-Coated Optical Fiber for Distributed Corrosion Monitoring in Soil and Aqueous Environments

aqueous environment↗

NASA NTRS2015

Characterization of Encapsulated Corrosion Inhibitors Containing Microparticles for Environmentally Friendly Smart Coatings

This poster presents the results obtained from experiments designed to evaluate the release properties, as well as the corrosion inhibition effectiveness, of several encapsulated corrosion inhibitors. Microencapsulation has been used in the development of environmentally friendly multifunctional smart coatings. This technique enables the incorporation of autonomous corrosion detection, inhibition and self-healing functionalities into many commercially available coating systems. Select environmentally friendly corrosion inhibitors were encapsulated in organic and inorganic pH-sensitive microparticles and their release in basic solutions was studied. The release rate results showed that the encapsulation can be tailored from fast, for immediate corrosion protection, to slow, which will provide continued long-term corrosion protection. The incorporation of several corrosion inhibitor release profiles into a coating provides effective corrosion protection properties. To investigate the corrosion inhibition efficiency of the encapsulated inhibitors, electrochemical techniques were used to obtain corrosion potential, polarization curve and polarization resistance data. These measurements were performed using the free as well as the encapsulated inhibitors singly or in combinations. Results from these electrochemical tests will be compared to those obtained from weight loss and other accelerated corrosion experiments.

Coatings↗

DOE OSTI2023

Corrosion of Al-Fe self-pierce riveting joints with multiphysics-based modeling and experiments

Self-piercing riveting (SPR) is an extensively used joining technique to assemble dissimilar materials. However, this joining of the dissimilar materials can generate galvanic/crevice corrosion, which can drastically impact the mechanical properties and the service life of the joint. In this study, a multiphysics-based hybrid modeling approach is developed for the galvanic corrosion of the Al-Fe SPR joints, which can consider the corrosion initiation and corrosion evaluation jointly. Experimental studies are first performed to extract information regarding the corrosion initiation sites, corrosion evolution and overall corrosion induced material loss in SPR joints. The initiation information is then passed onto the multiphysics FE model thus making it a hybrid model. This model can help understand the influences of metal microstructure on the corrosion propagation while the morphology changes can also be analyzed. Using the developed hybrid modeling approach, thorough parametric studies can be performed to explore the coupled impacts of multiple corrosion factors on the corrosion behavior of the joints. The developed hybrid model is validated on the prediction of galvanic corrosion for the SPR joints by comparing with experimental observations.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Liquid Interfacial Electron Microscopy Identifies Nanogalvanic Corrosion in Pearlitic Steel

The nanoscale mechanisms of localized corrosion in low carbon steels have remained elusive due to the complexity of studying the degradative material behavior at nanoscale solid-liquid interfaces. We identified various steps in the nanogalvanic corrosion processes using in-situ liquid-cell scanning transmission electron microscopy (STEM) using a microfluidic holder by Hummingbird Scientific. Initial work, performed at low magnification, identified the initiation point on a 1018 low-carbon steel surface. This initiation point was determined to be a triple junction of two ferrite grains bridging a cementite grain in contact with a baseline electrolyte of 6 uM CO2 dissolved in a buffered (2.78 uM Na2SO4) aqueous solution, pH 6.1. The pre-etched low-carbon steel surface was prepared using focused ion beam lift-out procedures to extract a cross-section of the low-carbon steel surface, which then was thinned to about 150 nm and transferred to a SiN membrane microfluidic window. The transfer was made using a lift-out needle to attach the low-carbon steel lamella to the corner of the SiN window, and then Pt/C deposition held the lamella in contact with the window while it was released from the lift out needle. To identify the triple point on the low carbon steel lamella, prior to attachment on the SiN window, the sample was characterized for compositional variations with energy dispersive x-ray spectroscopy mapping, grain orientation and phase mapping with precession electron diffraction, and thickness mapping with energy filtered transmission electron microscopy. This pre-characterization prior to the in-situ experiment provided a map of the multiphase and multigrain structure, where the in-situ liquid cell imaging provided a clear understanding of the initiation point on the sample. These data were cross-correlated to paint a holistic picture of the triple junction site, enabling low electron-fluence in-situ snapshot imaging to avoid dominating the native corrosion reactions with effects from the incident electron beam. This initial result identified that localized, nanogalvanic corrosion at the phase interface was the dominant corrosion process in the low-carbon steel, so we next targeted the observation of an array of these nanogalvanic features phase boundaries in a pearlite grain. Near-surface ferrite/cementite phase interfaces that typify pearlitic low-carbon steel were extracted, pre-characterized, and imaged for the in-situ corrosion processes. The sample was a cross-section from a pearlite grain, with alternating ferrite and cementite grains that extended microns down from the pre-etched low-carbon steel pipe surface. After contact with a buffered aqueous solution, the phase boundaries between the ferrite and cementite began to dissolve, with observable material loss and thickness changes in the dark-field and bright-field STEM images. Within minutes, the corrosion front proceeded deeper into the material, claiming a thin layer of ferrite around all exposed phase boundaries before progressing laterally into the ferrite matrix, converting the ferrite to corrosion product normal to each buried cementite grain. Formation of the corrosion product causes a volumetric expansion, creating a lateral wedging force that mechanically ejects the cementite grains from their grooves and leaves behind percolation channels into the steel substructure. Rapid and deleterious, this nanogalvanic corrosion pathway represents an important target for understanding and preventing run-away degradation in this common building material. Observation of this corrosion mechanism was enabled by the combination of pre-characterization using standard structural, grain, and compositional analysis in the TEM, which provides maps for understanding the reaction propagation captured in low-dose, in-situ, liquid-cell STEM.

corrosion↗

DOE OSTI2022

Uncertainty Quantification for Dissimilar Material Joints Under Corrosion Environment

Abstract Self-Piercing Riveting (SPR) is one of the most commonly used methods for joining dissimilar materials in the automotive industry. These joints are popular due to their adaptability, high performance and short cycle time. However, since these joints involve two dissimilar materials, they are susceptible to galvanic corrosion in the presence of an electrolyte which is driven by the difference in the equilibrium potential of the metals. This can affect the safety and resilience of these joints. In this paper, we focus on galvanic corrosion in Al-Fe SPR joints. A Machine learning (ML) based surrogate model, which is based off of FE simulations, for statistical corrosion analysis is developed. This model enables the resilience and reliability analysis of SPR joints under corrosion environment. In this study, first a physics-based finite element (FE) corrosion model has been developed to simulate the galvanic corrosion between a Fe cathode and an Al anode of a SPR joint. This model takes into account the effect of the crystal microstructure of the Al anode and the precipitation of the corrosion product. Several geometric and environmental factors including crevice gap, roughness of anode, conductivity, pH and the temperature of the electrolyte that effect corrosion are investigated. A thorough Uncertainty Quantification (UQ) analysis is conducted for the overall corrosion behavior of the Fe-Al SPR joints using a novelistic Probabilistic Confidence-Based Adaptive Sampling (PCAS) technique. PCAS is used to train the surrogate model by identifying the critical sampling points and thus reducing the overall computational costs. It is found that the electrolyte temperature has the largest effects on the material loss and needs to be managed closely for better corrosion control. By understanding the corrosion performance and resultant uncertainty impact on SPR joints, the reliability and resilience of these joints can be improved.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Predicting and Controlling Corrosion (Abbreviated Final Report)

Corrosion accumulates significant replacement costs in the transportation, utility, manufacturing, and infrastructure sectors. It also underpins several of LLNL’s core missions in stockpile stewardship, defense, and energy security. Whereas most corrosion and aging models are empirically parameterized to describe well-defined conditions late in the reaction, the factors that determine the early stages of corrosion—during which mitigation could be most impactful— are poorly understood. This project addressed the critical need for new approaches to predict the kinetics of corrosion initiation based on firm physical and chemical understanding. The activities encompassed degradation of relevant metals in both hydrogen-rich and environmental corrosion scenarios. The team integrated state-of-the-art multiscale simulation, in situ characterization, and data science within three technical thrusts: hydriding of Ti alloys; aqueous corrosion of Al and Ni-Cr alloys; and degradation of additively manufactured 316L stainless steel. In each case, novel capabilities were developed to identify and track the impacts of key atomistic, compositional, and microstructural features on the metal systems. For hydriding, protocols were developed to tightly integrate multiscale models, advanced multimodal characterization, and machine learning to determine how hydrogen interacts with native passivating surface oxides and nucleates new undesired phases, shedding new light on the critical role of grain boundaries, interfaces, and atomically disordered regions. For aqueous corrosion, the project demonstrated methods to predict dissolution rates of metal surfaces in corrosive solutions, to measure and understand microstructural and grain orientation effects on corrosion susceptibility, and to investigate competing growth and dissolution kinetics of surface oxides. For additively manufactured metals, analysis using state-of-the-art microscopy techniques revealed the role of specific heterogeneities invoked during laser processing, including cellular structure, dislocations, and precipitates, on corrosion susceptibility. In addition to new capabilities and understanding, the project provided an avenue for workforce development, as well as key partnerships with stakeholders in corrosion science.

08 HYDROGEN↗