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DOE OSTI2019

Effect of pH on Corrosion Performance of Cu-Se and Cu-Se-Te Alloys in 3.5% Sodium Chloride Solution

The influence of pH (2, 7, 12) on the corrosion behavior of Cu-Se-Te and Cu-Se alloys in a 3.5% sodium chloride solution was investigated using static immersion testing and electrochemical methods. The morphologies of the alloys after corrosion were observed by scanning electron microscopy. The distribution of elements was detected by energy-dispersive spectrometry, and the phases were identified by x-ray diffraction. The results indicate that the corrosion rate decreases significantly with an increase in pH. No compact protective film forms on the alloy surface when pH is 2; meanwhile, Cu{sub 2}(OH){sub 3}Cl and Cu{sub 2}O films form on the alloy surface when pH is 7 or 12. The corrosion rates of alloys in the NaCl solution with different pH levels vary because the cathode reaction and the protective films affect the corrosion rate synthetically. In addition, the Cu-0.5Se alloy generally exhibits satisfactory conductivity, strength, and corrosion resistance. The corrosion resistance of the Cu-0.5Se alloy is higher than that of the Cu-Se-Te alloys, particularly at low pH levels.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Effect of MgCl{sub 2} on the Corrosion Behavior of Copper Under Periodic Wet/Dry Cycle Condition

The corrosion behaviors of copper under periodic wet/dry cycle conditions were investigated. The characteristics of the corrosion product formed on copper were analyzed by x-ray diffraction, scanning electron microscopy, energy-dispersive spectroscopy, and in situ electrochemical impedance spectroscopy. Weight loss results showed that the corrosion of copper under an MgCl{sub 2} deposition condition was more severe than that under NaCl. The main corrosion products formed on the tested sample under NaCl deposition condition consisted of Cu{sub 2}Cl(OH){sub 3} and Cu{sub 2}O, while those under the MgCl{sub 2} deposition condition consisted of Cu{sub 2}Cl(OH){sub 3} and Mg{sub 2}(OH){sub 3}Cl·4H{sub 2}O. In the case of the NaCl deposition condition, a two-layered structure formed during the corrosion process. However, the corrosion product layer formed on copper under the MgCl{sub 2} deposition condition had an extremely loose structure. The effect of MgCl{sub 2} on the corrosion mechanism of copper is discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Hot Corrosion Performance of Single-Crystal CMSX-4 and CMSX-486 Superalloys in the Mixture of Na{sub 2}SO{sub 4}-NaCl Melts

A modification in the chemistry of single-crystal CMSX-4 to produce CMSX-486 superalloy has been reported in the literature to be accomplished without degradation in high-temperature mechanical performance. However, adequate attention has not yet been focussed on the hot corrosion response of the alloy considering its chemical composition modification. This paper reports for the first time that a considerable degradation in the hot corrosion resistance of CMSX-4 occurs by the modification of its chemistry. Corrosion tests at different salt concentrations and temperatures showed that the hot corrosion resistance of CMSX-486 is worse than the conventional CMSX-4 alloy. The difference in the corrosion resistance characteristics of the two alloys is attributable to the nature of the protective oxide layer formed on the materials during hot corrosion. Characterization using various advanced techniques revealed that the oxide layer formed on CMSX-486 consists of less amount of protective and coherent Al{sub 2}O{sub 3} and Cr{sub 2}O{sub 3} film than CMSX-4, and this is the reason for its poor hot corrosion resistance.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Composite coatings from polycarbosilane derived SiC and Al/SiC cermet active fillers as protective barriers against steel corrosion

Stainless steel is used throughout the world as a structural material. However, it undergoes corrosion damage when exposed to extremely corrosive media, such as the marine environment. An alternative to solve this problem lies in the development of coatings that can withstand extreme conditions but also be easily deposited with inherently corrosion-resistant materials such as silicon carbide (SiC). The present study shows a simple method to produce Al/SiC cermet powders by attrition milling. The resulting cermet powders with a metallic matrix and hemispherical morphology, were employed as fillers in polycarbosilane (PCS) solutions that were sprayed on A304 stainless steel substrates. Al/SiC composite coatings were produced after heating the sprayed suspensions at 700 °C for 1 h in Ar atmosphere. The resulting composite coatings exhibited low surface energies (< 35 mN/m), water contact angles of 53°, and adhesion strength of up to 30 MPa. Finally, corrosion tests were performed in a cyclic corrosion test chamber, showing that these coatings effectively reduced the corrosion rate of stainless steel by 87%, reaching corrosion rate values of 0.007 g/cm 2 year.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Development of chloride-induced corrosion in pre-cracked RC beams under sustained loading: Effect of load-induced cracks, concrete cover, and exposure conditions

This paper deals with corrosion initiation and propagation in pre-cracked reinforced concrete beams under sustained loading during exposure to a chloride environment. Specimen beams that were cast in 2010 were compared to specimens cast in 1984. The only differences between the two sets of beams were the casting direction in relation to tensile reinforcement and the exposure conditions in the salt-fog chamber. The cracking maps, corrosion maps, chloride profiles, and cross-sectional loss of one group of two beams cast in 2010 were studied and their calculated corrosion rates were compared to that of beams cast in 1984 in order to investigate the factors influencing the natural corrosion process. Experimental results show that, after rapid initiation of corrosion at the crack tip, the corrosion process practically halted and the time elapsing before corrosion resumed depended on the exposure conditions and cover depth.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Chloride-induced corrosion mechanism and rate of enamel- and epoxy-coated deformed steel bars embedded in mortar

The chloride-induced corrosion mechanisms of uncoated, pure enamel (PE)-coated, mixed enamel (ME)-coated, double enamel (DE)-coated, and fusion bonded epoxy (FBE)-coated deformed steel bars embedded in mortar cylinders are investigated in 3.5 wt.% NaCl solution and compared through electrochemical tests and visual inspection. Corrosion initiated after 29 or 61 days of tests in all uncoated and enamel-coated steel bars, and after 244 days of tests in some FBE-coated steel bars. In active stage, DE- and FBE-coated steel bars are subjected to the highest and lowest corrosion rates, respectively. The uncoated and ME-coated steel bars revealed relatively uniform corrosion while the PE-, DE-, and FBE-coated steel bars experienced pitting corrosion around damaged coating areas. Due to the combined effect of ion diffusion and capillary suction, wet–dry cyclic immersion caused more severe corrosion than continuous immersion. Both exposure conditions affected the corrosion rate more significantly than the water–cement ratio in mortar design.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Validating corrosion models: Influence of physical properties

In chloride containing environments, two metals in physical contact can undergo galvanic corrosion limiting the lifetime of components. Being able to accurately predict galvanic corrosion damage distributions over time has not been widely presented in literature. Therefore, Finite Element Method (FEM) corrosion models were experimentally validated for two galvanic couples as a function of governing equations, environment, anode material, anode:cathode ratio, and time. Carbon steel/stainless steel (CS/SS) and zinc/stainless steel (Zn/SS) galvanic couples were exposed to NaCl solutions at room temperatures for up to 14 days. For the galvanic couples and environments, the Laplace equation with variable conductivity and reactions was sufficient to model the experimental corrosion damage. Increasing the chloride concentration for the CS/SS galvanic couple, regardless of the anode:cathode ratio, decreased the observed and modeled corrosion damage. Decreasing the anode:cathode ratio (i.e., increasing the cathode length), increased the experimentally observed and modeled corrosion damage. For small anode:cathode ratios, the governing equations deviate over long time periods with the Nernst-Plank equation being conservative. For the Zn/SS galvanic couple, the cathode length controls the dominant cathodic reduction reaction. For small cathode lengths, the hydrogen evolution reaction is dominant. For larger cathode lengths, the oxygen reduction reaction is dominant. The results are discussed with regard to the influence of solution chemistry, ohmic drop, and governing reactions. Overall, validated FEM models were presented, and the resultant models, physics, and mechanisms can be applied to other corrosion scenarios with confidence.

Carbon steel↗

DOE OSTI2023

Effect of chromium on corrosion resistance of Ni-Cr-Mo-Gd alloys in seawater

Neutron absorbing materials are being considered within commercial spent nuclear fuel disposal canisters to maintain nuclear subcriticality in storage. To select candidate alloys for the canisters, both neutron absorption and corrosion resistance should be considered. This work examines corrosion resistance of Ni-Cr-Mo-Gd alloys developed specifically for neutron absorption. The addition of Gd results in a secondary gadolinide phase (Ni 5 Gd) that significantly changes the corrosion properties. Testing was performed primarily in seawater at 30°C. Seawater was selected as the most prevalent terrestrial brine and is characterized by a high chloride concentration. Various electrochemical corrosion techniques were carried out to evaluate Ni-Cr-Mo-Gd alloys with different Cr compositions and investigate the role of Ni 5 Gd phase on corrosion behavior. C22 was included as a benchmark material, due to the similarity in composition and the significant corrosion data available. Here, test results showed a tendency to passivate over time which is attributed to dissolution of surface exposed Ni 5 Gd phase. Cross-sectional analysis indicated that dissolution could penetrate hundreds of micrometers deep under aggressive conditions. It was found that higher Cr variant (21.01%) showed much shallower impact, suggesting Cr prevented primary phase corrosion and thus reduced Ni 5 Gd phase dissolution. Acid pickling of the specimens showed much less dissolution for a higher Cr material and suggested some primary phase dissolution for the low Cr specimen. Acid pickled specimens showed positive shifts in the repassivation potential, suggesting increased surface passivation.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2018

Simultaneously improving mechanical properties and corrosion resistance of pure Ti by continuous ECAP plus short-duration annealing

Highlights: • Additional short-time annealing led to enhanced strength of UFG Ti due to texture strengthening. • UFG Ti showed improved corrosion resistance in artificial seawater compared with initial CG Ti. • Short-duration annealing enhanced corrosion resistance of UFG Ti due to stronger basal texture. - Abstract: This work investigated the effect of short-duration annealing on mechanical properties and corrosion behavior of bulk ultrafine-grained (UFG) pure Ti (grade 2) produced by high-efficiency equal-channel angular pressing (ECAP), serving the fast developing of marine industries. The initial coarse-grained (CG) Ti achieved higher strength after continuous ECAP at 420 °C for 4 passes, while additional short-duration annealing at 300 °C for 15 min of UFG Ti further led to extraordinary improvement of strength, which was associated with texture strengthening. The yield strength was increased from 362 MPa in as-received state to 561 MPa in post-ECAP annealed condition, and ultimate tensile strength from 450 MPa to 663 MPa. The ECAP-processed UFG Ti had better corrosion resistance in artificial seawater than the initial CG Ti. Short-duration annealing further improved the corrosion resistance of UFG Ti, which was related to stronger basal texture. The corrosion current density decreased from 68.37 nA cm{sup −2} for CG Ti in as-received condition to 41.77 nA cm{sup −2} for UFG Ti processed by ECAP plus short-duration annealing. The fraction of TiO{sub 2} within the surface oxide film for the post-ECAP annealed sample was increased. The bulk UFG Ti after post-ECAP short-duration annealing revealed an excellent combination of high strength, good ductility and superior corrosion resistance for marine applications.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Advanced neutron absorber Ni-Cr-Mo-Gd alloys seawater corrosion mechanism and susceptibility study

Previous studies demonstrated the corrosion susceptibility of advanced neutron absorber (ANA) Ni-Cr-Mo-Gd in a seawater environment but remained inconclusive. In this paper, scanning electron microscopy was employed to identify the corrosion phase in Ni-Cr-Mo-Gd, and computational thermodynamic simulation was used to study phase corrosion potentials. Results showed that the Ni 5 Gd second phase, distributed along FCC grain boundaries in Ni-Cr-Mo-Gd, has lower corrosion potential than the substrate. Furthermore, heat treatment and alloy chemistry adjustment would not ameliorate the ANA corrosion susceptibility. Finally, isolating the Ni 5 Gd from the corrosion medium through advanced manufacturing is a viable way to improve the ANA corrosion resistance.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Progress and opportunities in corrosion mitigation in heat transfer fluids for next-generation concentrating solar power

Concentrating solar power (CSP) systems have gained considerable eminence in converting solar thermal energy into electrical power in recent years. According to the U.S. Department of Energy's Gen3 roadmap, the CSP system should operate > 700 °C, as its efficiency depends directly on the operating temperature of the heat transfer fluids (HTFs). A significant challenge, however, is the corrosion of containment materials by the HTFs that is exacerbated at the higher temperatures. A comprehensive review of the high temperature stable HTFs, their properties, corrosion mechanisms on different alloys, and corrosion mitigation measures is of much importance for directing a concerted research and development in the field, which forms the motivation for this compendium. First, molten salt HTFs and their thermophysical properties, along with liquid metals, are introduced. Corrosion of structural materials in different HTFs including molten salts, liquid metals, and supercritical carbon-di-oxide at various temperatures and the corrosion mechanisms are comprehensively reviewed. In addition, several corrosion mitigation methods are discussed. Finally, future directions for HTFs and corrosion mitigation methods in molten salts are proposed. As a result, the holistic review presented here will serve as the foundation for further research addressing relevant challenges and enabling the promise of achieving cost-competitive CSP.

14 SOLAR ENERGY↗

DOE OSTI2021

Dispersion curve regression – assisted wideband local wavenumber analysis for characterizing three-dimensional (3D) profile of hidden corrosion damage

Corrosion as common damage in civil, petrochemical, nuclear, and aerospace structures affects the integrity and safety of the structures and may lead to catastrophic failures. This paper presents dispersion curve regression-assisted local wavenumber analysis method, which can analyze the time–space wavefield containing wideband information of wave-damage interaction and further extract the structural information carried by such wavefield for characterizing hidden corrosion damage in an isotropic plate. To acquire the time–space wavefield, a noncontact scanning laser Doppler vibrometer is used. In our analysis method, the acquired time–space wavefield is firstly processed to generate a local wavenumber function. The derived wavenumber function is further analyzed with a dispersion curve regression step, which searches in a set of theoretical frequency-wavenumber dispersion curves for different plate thicknesses and identifies the optimal plate thickness whose theoretical curve best matches the frequency-wavenumber relation contained in the local wavenumber function. By this means, a 3D profile including both in plane and thickness dimensions of the structure can be constructed for corrosion visualization and quantification. The experimental study demonstrates that our method can quantify the profile of hidden uniform corrosion in metal plates in terms of its in-plane shape and size as well as its out-of-plane depth in the subwavelength scale. Moreover, compared to previous Lamb wave-based corrosion inspection methods, our technique allows for noncontact 3D characterization of hidden corrosion from a far distance to the structure. Finally, we believe this work will inspire new 3D damage quantification methods that are based on wavefield analysis as well as enable potential applications for the quantification of hidden corrosion in civil, petrochemical, nuclear, and aerospace structures.

42 ENGINEERING↗

DOE OSTI2018

Effects of Chlorine in Ash on the Corrosion Performance of Ni-Based Alloys in a Simulated Oxy-Fuel Environment

Coal ash can severely attack alloy materials at high temperature. To understand coal ash corrosion, a critical study is needed to determine the effect of the elements in ash on corrosion and find an approach to reduce the corrosion rates in an ash environment at high temperature. Chlorine is a harmful element in coal. The role of chlorine in ash corrosion is investigated in simulated oxy-fuel environments. Long time tests up to 3000 hours were performed on various structural alloys at 750°C. Detailed results are presented on weight change, scale thickness, internal penetration, microstructural characteristics of corrosion products, and the cracking of scales for the alloys after exposure at 750°C for 3000h. In addition, we performed synchrotron nanobeam Furthermore X-ray analysis to study the phase and chemical composition of the oxide layers on the alloy surface. Results from these studies are used to address the role of chlorine in ash in the long-term corrosion performance of alloys. Nanobeam X-ray and SEM analyses indicate that chlorine can modify the diffusion mechanism near alloy surface, and increase corrosion rate.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Corrosion Susceptibility of Cr–Mo Steels and Ferritic Stainless Steels in Biomass-Derived Pyrolysis Oil Constituents

In this work, to better understand and evaluate the corrosion performance of candidate structural steels and ferritic stainless steels for production, transport, and storage of biomass pyrolysis oils, corrosion studies were conducted in selected organic constituents of bio-oils, including catechol, formic acid, and their mixtures as well as lactobionic acid, using electrochemical impedance spectroscopy. R 2 , the resistance against corrosion reaction, was obtained by fitting measured impedance spectra into an equivalent circuit. The values of R 2 were then used to assess corrosion resistance of the steels in each organic constituent and mixture. Type 410 and 430 stainless steels were resistant to corrosion in all tested organic constituents, while 2.25Cr-1Mo steel was not. 9Cr-1Mo steel was corrosion resistant in catechol but not in the other mixtures that contained organic acids. On the basis of the results of this work, it is suggested that the corrosion resistance against organic acids is attributed to formation of a Cr-rich passive film that requires stainless steels with critical Cr levels in excess of approximately 11 wt %. In catechol-only solution, lower levels of Cr intermediate between that of 2.25Cr-1Mo steel and 9Cr-1Mo steel appeared sufficient.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Electrochemical Corrosion and Catalysis Dynamics of Tin Oxide during Water Oxidation

Metal oxide corrosion severely limits anodic electrocatalysis, particularly at high potentials in acidic environments, where degradation pathways remain poorly defined. This study establishes explicit connections between corrosion and electrocatalysis on tin oxide during water oxidation by examining the roles of lattice defects, reactive oxygen species, interfacial pH variations, and speciation of corroded tin in acid. We first demonstrate the presence of structural defects such as oxygen vacancies and substoichiometric Sn(II) species by integrating electron paramagnetic resonance spectroscopy, ultraviolet photoelectron spectroscopy, and Mott–Schottky analysis. Kohn–Sham density functional theory calculations reveal that explicit water structures thermodynamically stabilize reaction intermediates and lower reaction overpotentials. Moreover, we propose that water dissociation leads to hydrogen-bonding networks formed by H* and OH* intermediates, which may span the entire catalyst surface and decrease the interfacial pH to drive corrosion. In contrast, the electrochemical generation of reactive oxygen species is shown to play a minor role in catalyst corrosion during water oxidation using inductively coupled plasma mass spectrometry coupled with selective chemical scavengers. Square-wave voltammetry combined with rotating ring-disk electrodes is used to reveal that under open-circuit conditions, only Sn(IV) cations chemically dissolve from tin oxide, while both Sn(IV) and Sn(II) species electrochemically corrode during water oxidation. Our results unveil a dynamic and complicated interplay between corrosive and catalytic pathways on metal oxide electrocatalysts: a decrease in interfacial pH due to water oxidation exacerbates Sn(II)/Sn(IV) corrosion. Subsequently, the electrochemical corrosion of Sn(II)/Sn(IV) facilitates product formation from lattice oxygen, while the redeposition of corroded Sn(II) as Sn(IV) can enable oxygen exchange with water. By elucidating the roles of defects and interfacial chemistry, this work provides a roadmap for engineering improved electrocatalysts that balance activity and stability, a critical step toward scalable and durable energy technologies.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Nanoscale morphological evolution of monocrystalline Pt surfaces during cathodic corrosion

This paper studies the cathodic corrosion of a spherical single crystal of platinum in an aqueous alkaline electrolyte, to map out the detailed facet dependence of the corrosion structures forming during this still largely unexplored electrochemical phenomenon. We find that anisotropic corrosion of the platinum electrode takes place in different stages. Initially, corrosion etch pits are formed, which reflect the local symmetry of the surface: square pits on (100) facets, triangular pits on (111) facets, and rectangular pits on (110) facets. We hypothesize that these etch pits are formed through a ternary metal hydride corrosion intermediate. In contrast to anodic corrosion, the (111) facet corrodes the fastest, and the (110) facet corrodes the slowest. For cathodic corrosion on the (100) facet and on higher-index surfaces close to the (100) plane, the etch pit destabilizes in a second growth stage, by etching faster in the (111) direction, leading to arms in the etch pit, yielding a concave octagon-shaped pit. In a third growth stage, these arms develop side arms, leading to a structure that strongly resembles a self-similar diffusion-limited growth pattern, with strongly preferred growth directions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

The role of gamma radiation on zircaloy-4 corrosion - 2016-0029

A key microstructural feature of irradiated oxide films that form on Zircaloy-4 is the development of significant amounts of interconnected porosity or microcracking, particularly along oxide grain boundaries. This development disrupts the protective nature of the barrier layer, effectively resulting in an increase in the observed post-transition corrosion rates. This observation suggests that some aspect of oxide dissolution may be occurring. It is noteworthy that when exposed to photons with energies greater than that of the oxide band gap, n-type semiconducting oxides are prone to dissolution. Because zirconia (ZrO{sub 2}) is an n-type semiconductor, it is plausible that high-energy photons may play an important role in corrosion. In an operating nuclear reactor, neutron and gamma flux levels are closely interrelated because they arise, for the most part, from the same originating process (i.e., the fissioning of nuclear fuel). Thus, it is difficult to isolate the independent effects of neutron and gamma radiation on corrosion. It is, however, theoretically conceivable to assess the role that gamma radiation may have on corrosion by comparing instances where variations in radiation environment exists; specifically by comparing where variations in gamma flux levels relative to neutron flux levels within different regions of a reactor or from reactor to reactor exist. Comparisons of the corrosion rates obtained between two different reactors (the Halden test reactor and the advanced test reactor [ATR]) that have differing gamma-to-neutron ratios were performed. In addition, an examination of corrosion rate data from the ATR, in which a variation in gamma-to-neutron flux ratio exists, was also conducted. Results are presented, from both assessments, which indicate that gamma radiation plays a role in the irradiated corrosion behavior of Zircaloy-4. In addition to a discussion of experimental data, potential mechanisms associated with photon-induced oxide dissolution of n-type semiconducting oxides, such as zirconia, is also provided. (authors)

36 MATERIALS SCIENCE↗

DOE OSTI2016

Effects of chemistry and microstructure on corrosion performance of Zircaloy-2-based BWR cladding - 2016-0066

In boiling water reactors (BWRs), Zircaloy-2 is typically the material of choice for fuel cladding. With increased focus on fuel performance and reliability, consistent cladding corrosion performance under varying BWR conditions has become an acknowledged requirement for modern BWR fuel. To support optimization of corrosion performance, modifications to alloy chemistry and manufacture conditions can be made, supported by ex-reactor corrosion testing and demonstrated through in-reactor operation. In this work, the combined effects of alloy chemistry and fabrication process were investigated. The effect of alloy chemistry is often complicated by variation within a production ingot. In this work, additional measurements were intentionally taken at the tube-shell stage (before cold pilgering) so that chemistry more representative of the final cladding could be obtained and the effect of iron, nickel, and tin could be examined more closely. Although chemistry range of Zircaloy-2 was the primary focus, the effect of iron above the ASTM limit in a new alloy was also explored. Three types of cladding fabrication processes were considered. Two types included a heat treatment applied after the first cold pilgering and annealing, and the treatment was limited to the outer portion of the cladding and differed in the temperature of the heat treatment; the third type had no special heat treatments after the first cold pilgering and annealing. The weight gain of the three types of cladding with varying compositions under two corrosion test conditions (400 deg. C steam and 410/520 deg. C two-stage steam) are discussed in terms of the initial second-phase particle sizes obtained from transmission electron microscopy examinations. Based on poolside inspections and hot-cell examinations, the in-reactor corrosion performance of the two cladding types up to typical discharge exposures are discussed in the terms of corrosion margin, microstructure evolution, and correlation with ex-reactor corrosion test data. (authors)

36 MATERIALS SCIENCE↗