Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Organisationseinheit der BAM
- 7.6 Korrosion und Korrosionsschutz (54) (entfernen)
The copper alloyed stainless steel 1.4542 (X5CrNiCuNb16-4) is used in different areas due to its good mechanical properties and corrosion resistance. Strength and corrosion resistance can be adjusted by the heat treatment, which is of importance for the application of this alloy. The mechanical properties (strength and hardness) are attributed to the dispersive precipitation of the copper rich ε–Phase. The additional precipitation of chromium carbides can reduce the corrosion resistance. Different ageing states were produced to investigate the precipitation behaviour with various methods. Furthermore, the influence of cold-rolling on the precipitation behaviour was studied in comparison to a solution annealed state without deformation. The microstructure was studied by SEM and the variations of hardness and magnetic proportion were characterised. The electrochemical potentiodynamic reactivation
(EPR) was used to determine the corrosion resistance and detect chromium depletion in all heattreated states. The results show that a work hardening accelerates the precipitation rate, while ageing at 600 °C reduces the corrosion resistance due to chromium depletion.
Aging of passive film formed on UNS N08031 was investigated as a function of passivation time in Green-Death solution at 40°C. The specimen surface was in a stable passive state in the solution.
The passive current density increased with an increase in the passivation potential. Electrochemical Impedance Spectroscopy and Mott–Schottky (M–S) analyses revealed that a more defective n-type
semiconductive passive film formed as the potential increased while the film became stable as the defects in the film decreased at potential lower than 1.0 VSSE. The increase of the applied potential and the polarisation time are likely reasons for the change in passive film stability.
Nickel‐free high‐nitrogen‐alloyed stainless steels like the P2000 (X13CrMnMoN18‐14‐3) were developed to enhance the strength and corrosion resistance of austenitic stainless steels like 304 and 316 while keeping the typical high ductility. The mechanical and corrosive properties of P2000 were investigated and compared with 304 and 316 to highlight the application opportunities of this new alloy. The microstructure of the solution‐annealed condition was characterised by electron backscatter diffraction and the mechanical properties were studied by uniaxial tensile tests, Charpy impact tests and hardness measurements. The passivation behaviour was analysed using the electrochemical potentiodynamic reactivation, whereas the pitting corrosion resistance was compared by pitting potentials and pitting temperatures. However, secondary thermal influences or suboptimal heat treatment can impair the corrosion resistance due to the precipitation of secondary phases and the resulting sensitisation. Thermodynamic calculations and artificial ageing treatment in the range of 500–900°C for up to 100 h were used to determine critical time–temperature parameters for sensitisation. The microstructure of the various aged states was evaluated by scanning electron microscopy and compared with the degrading corrosion resistance characterised by the KorroPad method.
Chloride contents at the steel–mortar interface that initiate steel corrosion were determined for carbon steel in alkali‐activated fly ash mortar for three different exposure conditions: exposure to 1 M NaCl solution; leaching in deionized water and then exposure to 1 M NaCl solution; and leaching in deionized water, aging in air at 20°C and natural CO2 concentration, and then exposure to 1 M NaCl solution. For comparison, a Portland cement mortar, exposed to 1 M NaCl solution, was studied. The median values of the corrosion‐initiating chloride contents (average over the full length of the rebar) in the alkali‐activated fly ash mortar varied between 0.35 and 1.05 wt% Cl with respect to binder, consistently lower than what was obtained for the Portland cement mortar, but with no clear trend regarding the exposure conditions. For most of the alkali‐activated fly ash mortar specimens, preferential corrosion at the connection between the working electrode and the external measurement setup was observed, while preferential corrosion did not occur for the Portland cement mortar. Scanning electron microscopy and auxiliary experiments in synthetic solutions indicated that this behavior was caused by inhomogeneities at the steel–mortar interface in the alkali‐activated mortar, likely due to its peculiar rheological properties in the fresh state.
Interfacial properties related to wettability and corrosion in CO2 transport pipelines are experimentally determined by the sessile and the pendant drop methods. The contact angle of a water drop in a compressed CO2 atmosphere is analyzed on an X70 pipeline carbon steel and compared to that on a martensitic steel S41500 to elucidate the effect of corrosion process on active wetting behaviour. The measurements are performed with liquid CO2 at 278 K and pressures ranging from 5 to 20 MPa. The results show that the contact angle (CA) increases with pressure from 132 ° to 143 ° for S41500 and from 117 ° to 137 ° for X70 and decreases with drop age by 20 ° to 24 ° regardless of the pressure and of the fact that corrosion only occurs on X70, which is confirmed by scanning electron microscopy, element mapping and energy dispersive x-ray spectrometry (EDS) analysis. At higher pressure, the contact angles on both materials converge. Further, related properties like density and interfacial tension were determined. CO2 - saturated water has a higher density than pure water: At 5 MPa saturated water reaches a density of 1017 kg⋅m^(-3) and at 20 MPa 1026 kg⋅m^(-3) compared to pure water with a density of 1002 kg⋅m^(-3) and 1009 kg⋅m^(-3), respectively. In this pressure range the IFT drops from 33 mN⋅m^(-1)at 5 MPa to 23 mN⋅m^(-1) at 20 MPa.
Geothermal energy is an interesting alternative to polluting fossil energy sources. Therefore, in Belgium, two wells have been drilled for a deep geothermal power plant. However, the environment to which the installations are exposed is challenging. The geothermal brine has 165 g/l total dissolved solids (of which 90% are sodium and chlorine) and the production temperature can be up to 130 °C. To assess their suitability to be used in a geothermal power plant, the corrosivity of the artificial brine to three common construction materials was investigated with exposure and electrochemical tests. The metals under consideration are a low-alloyed carbon steel (S235JR), an austenitic stainless steel (UNS S31603) and a duplex stainless steel (UNS S31803). The carbon steel, that was found to corrode uniformly, could be considered as a constructional material if a sufficient wall thickness is chosen. The austenitic stainless steel and the duplex stainless steel demonstrate very low uniform
corrosion rates. They are however susceptible to pitting and crevice corrosion. To guarantee safe operation of the geothermal power plant, the susceptibility of the alloys to stress corrosion cracking should be tested and in situ experiments should be performed.
A global transition towards more sustainable, affordable and reliable energy systems is being stimulated by the Paris Agreement and the United Nation's 2030 Agenda for Sustainable Development. This poses a challenge for the corrosion industry, as building climate‐resilient energy systems and infrastructures brings with it a long‐term direction, so as a result the long‐term behaviour of structural materials (mainly metals and alloys) becomes a major prospect. With this in mind “Corrosion Challenges Towards a Sustainable Society” presents a series of cases showing the importance of corrosion protection of metals and alloys in the development of energy production to further understand the science of corrosion, and bring the need for research and the consequences of corrosion into public and political focus. This includes emphasis on the limitation of greenhouse gas emissions, on the lifetime of infrastructures, implants, cultural heritage artefacts, and a variety of other topics.
The composites combining aluminum and silica nanoparticles with the addition of tetramethylammonium hydroxide (Al-SiO2(T)) and butanol (Al-SiO2(B)) as mixing media have been successfully fabricated. Corrosion behavior of Al-SiO2 composites before and after exposure in 1M NaCl solution was examined using potentiodynamic polarization (Tafel curve analysis). The study was also equipped with scanning electron microscopy (SEM), energy dispersive X-ray (EDX), and X-ray diffraction (XRD) investigations. Before exposure, Al-SiO2(T) exhibited the best corrosion resistance. Performance improvement was indicated by Al-SiO2(B) up to 10 times better than Al-SiO2(T) after exposure. The increased SiO2 content did not significantly enhance the corrosion resistance of the composites. The Al-SiO2 composites with 5% SiO2 content showed very high corrosion resistance (as the optimum composition). Furthermore, pitting corrosion was observed in the Al-SiO2 composites, indicated by the formation of corrosion products at grain boundaries. The product was affected by the presence of SiO2 in the Al matrix and the NaCl environment at 90 °C (approach to synthetic geothermal media: Na+, Cl, H+, OH-). Our study revealed the presence of γ-Al2O3, γ-Al(OH)3, and Al(OH)2Cl as the dominant corrosion products.
Hard coated steel components are used in a wide application range, mostly for protective, wear resistant and decorative purposes. Despite of these coatings being regarded as relatively dense, there is always a high risk of localized corrosion when a coated low alloyed steel component encounters a surrounding high humidity atmosphere or even an aqueous medium. An approach to enhance the corrosion properties is the addition of magnesium to physical vapor deposited hard coatings, like TiN. It has been found that there is a remarkable increase in corrosion resistance in dependence of magnesium content of the TiMgN coating and its surface properties. In this work the authors will explain the underlying corrosion protection mechanisms by means of electrochemical and analytical studies. The positive impact of magnesium in the coating relates on its preferred dissolution vs. steel. This causes the potential to shift to more negative direction with respect to the steel substrate and additionally leads to a temporarily passivation of the steel due to alkalization of the surrounding electrolyte by formation of magnesium hydroxide.
Hard and wear resistant coatings deposited by PVD techniques have been characterized for decades for their capabilities to protect steel substrates from corrosion. In the present work the effect of Mg incorporated into TiN coatings is described in terms of the corrosion behavior as well as the mechanical and structural properties.
TiN and TiMgN films with Mg contents between 10 and 35 at.% were deposited onto mirror polished 100Cr6 (1.3505) steel samples with 2.5 and 5 μm thickness by using DC magnetron sputtering. The corrosion protection capabilities of the coatings were characterized by neutral salt spray (NSS) test, considering the amounts and sizes of growth defects inherent in each coated sample as determined by a recently developed optical scan method (Large Area High Resolution mapping). The defect data were statistically analyzed for improved interpretation of NSS test results. Chosen growth defects were additionally analyzed by focused ion beam technique. Furthermore the coating composition and morphology, the hardness and the tribological behavior were characterized.
Polished steel samples coated with 2.5 μm TiMgN containing about 35 at.% Mg were in the plane free of corrosion after 24 h in a NSS test. TiMgN with 10 or 20 at.% Mg only provided a slightly improved corrosion protection in relation to pure TiN coatings, which was limited to certain types of growth defects. The highest Mg containing coatings exhibited a decreased hardness down to 1200 or 1800 HV depending on type of deposition (HV 1200: Ti- and Mg-target with rotating substrate holder, 1800: Mg-plugged Ti-target with static substrate holder), but also showed a strongly improved wear resistance against Al2O3 related to pure TiN. By analyzing the NSS test results it was found that the corrosion behavior of the coated samples did not only depend strongly on the Mg content, but also on the sample individual defect concentrations. Therefore this subject is extensively discussed.
For reliability and safety issues of injection wells, corrosion resistance of materials used needs to be determined. Herein, representative low-cost materials, including carbon steel X70/1.8977 and low alloyed steel 1.7225, were embedded in mortar to mimic the realistic casing-mortar interface. Two types of cement were investigated: (1) Dyckerhoff Variodur commercial Portland cement, representing a highly acidic resistant cement and (2) Wollastonite, which can react with CO2 and become stable under a CO2 stream due to the carbonation process. Exposure tests were performed under 10 MPa and at 333 K in artificial aquifer fluid for up to 20 weeks, revealing crevice corrosion and uniform corrosion instead of expected pitting corrosion. To clarify the role of cement, simulated pore water was made by dispersing cement powder in aquifer fluid and used as a solution to expose steels. Surface analysis, accompanied by element mapping on exposed specimens and their crosssections, was carried out to trace the chloride intrusion and corrosion process that followed.
Ageing at 600 °C (from 0.1 h up to 20 h) leads to the formation of precipitations at the ferrite-ferrite (α/α) and ferrite-austenite (α/γ) grain boundaries of the lean duplex stainless steel (LDSS) X2CrNiN22-2. This leads to sensitisation due to chromium depletion and decreased pitting corrosion resistance proven by the results of various electrochemical methods (DL-EPR and determination of CPT, Epit). These results were compared with the KorroPad method, which uses an agar-based gel-electrolyte for the detection of stainless steel surfaces prone to pitting corrosion. However, the standard configuration of the KorroPad showed no differentiation for the various ageing conditions. Therefore, modified versions of the KorroPad with two, five and ten times higher NaCl and potassium ferrocyanide III (K3[Fe(CN)6]) concentrations were successfully used to visualise the behaviour detected by DL-EPR, Epit and CPT. Therefore, the KorroPad method can also detect a microstructure related reduction of pitting corrosion resistance, which can drastically reduce the experimental effort to generate sensitisation diagrams for stainless steels.
Although zinc and zinc coatings have been widely used for corrosion protection for decades new zinc coatings are constantly being developed. Characterizing the corrosion protectiveness of these new coatings, however, should not be underestimated. While exposure tests are time intensive, cyclic tests can only be used for a very limited field of application. Thus, electrochemical measurements provide both an efficient and an effective alternative. Conventional aqueous bulk electrolytes influence the surface layers of a tested zinc coating and are therefore not reliable. Gel electrolytes, however, have evolved over the last few years, are minimally invasive and provide reliable results.
This work describes experiments with gel electrolytes made of agar. Unlike previous work, it proposes a composition of gel electrolyte for minimally invasive description of the protective power of naturally formed oxide layers on zinc and zinc coatings. Therefore, as a first part, the gel electrolyte made of agar is verified as a method for zinc and zinc-coated samples. Afterwards, this paper introduces the corrosion product layer resistance RL as a promising parameter to evaluate the protective power of zinc coatings. Results are verified with EIS and FTIR measurements. An example on a representative zinc coating demonstrates the practical application.
Anlagenbauteile aus nichtrostendem Stahl sind durch eine Passivschicht auf der Oberfläche vor Korrosion geschützt. Ist diese beschädigt oder unvollständig ausgebildet, geht der Schutz verloren. Produktionsausfälle und hohe Investitionen für Instandsetzungen können die Folge sein. Das KorroPad-Verfahren ist ein Schnelltest zur Qualitätskontrolle der Passivschicht. Er nimmt nur 15 Minuten in Anspruch.
The research focus of this study was set on the corrosion process of condensate as droplets on the surface of carbon steels (X52, X70) martensitic steel UNS S41500, and super austenite UNS N08031 in CO2 atmosphere with impurities at 278 K (to simulate the offshore transportation condition in a buried pipeline). The possibility of dew/droplet formation on the steel surface and wetting behavior of corresponding materials were evaluated by contact angle measurement in dense CO2 at 278 K. To observe the effect of impurities (SO2 and O2) on droplet corrosion process, exposure tests were carried out in the mixed atmosphere with a drop, 1 ‑ 10 µL in volume, of CO2 saturated ultra-pure water on steel surface. Comparable exposure tests were carried out with the same gas mixture and the same volume of water, as vapor, to observe the droplet formation and the corrosion process that follows. Effects of surface roughness on the droplet formation and its corrosion process were further studied and showed no significant role upon long time exposure. The results from droplet experiments were compared to those from the bulk electrolyte for the further recommendation on the quality control of gas stream along with the use of carbon steels as transport pipelines in CCS - Carbon Capture and Storage system.
Early Stage of Corrosion Formation on Pipeline Steel X70 Under Oxyfuel Atmosphere at Low Temperature
(2020)
The early stage of corrosion formation on X70 pipeline steel under oxyfuel atmosphere was investigated by applying a simulated gas mixture (CO2 containing 6700 ppmv O2, 100 ppmv NO2, 70 ppmv SO2 and 50 ppmv H2O) for 15 h at 278 K and ambient pressure. Short-term tests (6 h) revealed that the corrosion starts as local spots related to grinding marks progressing by time and moisture until a closed layer was formed. Acid droplets (pH 1.5), generated in the gas atmosphere, containing a mixture of H2SO4 and HNO3, were identified as corrosion starters. After 15 h of exposure, corrosion products were mainly X-ray amorphous and only partially crystalline. In-situ energy-dispersive X-ray diffraction (EDXRD) results showed that the crystalline fractions consist primarily of water-bearing iron sulfates. Applying Raman spectroscopy, water-bearing iron nitrates were detected as subordinated phases. Supplementary long-term tests exhibited a significant increase in the crystalline fraction and formation of additional water-bearing iron sulfates. All phases of the corrosion layer were intergrown in a nanocrystalline network. In addition, numerous globular structures have been detected above the corrosion layer, which were identified as hydrated iron sulphate and hematite. As a type of corrosion, shallow pit formation was identified, and the corrosion rate was about 0.1 mma−1. In addition to in-situ EDXRD, SEM/EDS, TEM, Raman spectroscopy and interferometry were used to chemically and microstructurally analyze the corrosion products.
Geothermal brines often contain high amounts of lead and copper ions that can precipitate as native Cu and Pb as consequence of galvanic corrosion when brines react with carbon steel materials. This contribution evaluates which materials could overcome the problem of galvanic corrosion at geothermal environment.
The behavior of these materials in water containing high chloride concentration (> 100 g/L NaCl) as well as various amounts of dissolved bCl2 and/or CuCl2 was characterized by electrochemical and exposure measurements.
Both methods reveal carbon steel suffers corrosion susceptibility, accompanied by Cu◦ and/or Pb◦ precipitation on the surface. Electrochemical measurements on stainless steels result in significant difference in corrosion and repassivation potentials (Ecorr = -189 mV, Erep = 70 mV), indicating a good corrosion resistance.
The corrosion behavior of galvanized steels and zinc components under atmospheric exposure depends mostly on the corrosion product‐based cover layer formation under the prevailing conditions. The use of agar‐based gel electrolytes makes it possible to use electrochemical methods to obtain a characteristic value from these cover layers that describe their current and future protective capacity. It is shown here that different states of galvanized steel can be distinguished very well under laboratory conditions and that this method is also suitable for use under practical conditions. Based on the characteristic values and assuming future time of wetness, it is very easy to draw up a forecast for the future corrosion rate, which provides plausible values.
Novel agar-based test electrolytes are used to perform electrochemical corrosion investigations on ZnFe and ZnNi binary as well as ZnFeMo ternary zinc coatings. The objectives of the electrochemical investigations include the characterization of the corrosion behavior, the description of the protective effect of the coatings as well as the investigation of the layer formation and degradation under artificial aging. ZnFe and ZnFeMo coatings are applied with varying iron content as well as an additional passivation layer, respectively, to study the effect on corrosion resistance. The results show that the protective effect of the coatings is not negatively influenced by different iron contents or the addition of molybdenum. Additional passivation of the ZnFe-containing coatings by means of a passivating agent leads to a significant improvement in the protective effect. Artificial aging leads to slight degradation of the additional passivation layer whereas coatings without post-treatment enhance their protective effect by the formation of corrosion product layers.
Electrochemical deposition of polyaniline on carbon steel for corrosion study in geothermal solution
(2019)
Polyaniline has been widely developed for many applications, e.g. sensor, supercapacitor components, electrochromic devices, and anticorrosion pigments. Although the addition of polyaniline pigment in organic coatings has been an alternative for corrosion protection in industrial applications, the protection mechanism is still not fully understood. Herein in this study, as a part of the development of polyaniline/silicon dioxide coating for geothermal application, polyaniline has been deposited electrochemically on carbon steel surface in oxalic acid medium and tested in geothermal solution to understand the contribution of polyaniline to the corrosion protection of a polyaniline-based composite in the geothermal system. To observe the surface/interface reaction between the electrolyte and electrode surface during the electrochemical polymerization, electrochemical impedance spectroscopy (EIS) was applied after each cycle. For corrosion study in the geothermal application, an artificial geothermal solution was used with the composition of 1,500 mg/l Cl⁻, 20 mg/l SO₄²⁻, 15 mg/l HCO₃⁻, 200 mg/l Ca²⁺, 250 mg/l K⁺, and 600 mg/l Na⁺, and pH 4 to simulate a geothermal brine found in Sibayak, Indonesia. An electrochemical measurement was performed by monitoring the open circuit potential over seven days, with the interruption by EIS every 22 hours. The experiments were performed at room temperature and 150 °C (1 MPa) in an oxygen-free environment. Impedance spectra showed a reduction of the total impedance value of approximately 10 times for specimens measured at 150 °C compared to the specimens measured at room temperature, suggesting a less stable layer at high temperature.