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  • 1.
    Chen, Zhuo Yuan
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Corrosion Science.
    The role of particles on initial atmospheric corrosion of copper and zinc: lateral distribution, secondary spreading and CO2-/SO2-influence2005Doctoral thesis, comprehensive summary (Other scientific)
    Abstract [en]

    The role of sodium chloride (NaCl) particles and ammonium sulfate ((NH4)2SO4) particles on the initial atmospheric corrosion of copper and zinc was investigated under in situ and ex situ conditions using microgravimetry, FTIR spectroscopy, ion chromatography, scanning electron microscopy with x-ray microanalysis and the scanning Kelvin probe. For the first time, in situ infrared spectra were collected on a micron level during particle induced atmospheric corrosion using a recently developed experimental set-up for in situ FTIR microspectroscopy. Lateral distribution of corrosion and reaction products on copper and zinc surfaces was determined and could be connected with the mechanisms of the initial particle induced corrosion. The recently discovered secondary spreading effect from NaCl electrolyte droplets on metal surfaces was studied under in situ conditions and the effect of CO2 on the spreading process was elaborated. The ambient level of CO2 (350 ppm, 1 ppm = 10-6 volume parts) results in a relatively low secondary spreading effect, whereas the lower level of CO2 (<5 ppm) causes a much faster secondary spreading effect over a large area. At low CO2 concentration alkaline conditions will prevail in the cathodic area, leading to large changes in the surface tension at the oxide/electrolyte interface in the peripherical parts of the droplet. This induces a surface tension driven convective flow of electrolyte from the NaCl droplet. The continuous growth of the secondary spreading area at low CO2 concentration is possible due to the galvanic coupling with the droplet leading to transport of sodium ions to this region and maintenance of the alkaline conditions. At 350 ppm CO2, carbonate formation in the secondary spreading area results in lowering of the pH, increasing the surface tension of the oxide/electrolyte interface and inhibiting the secondary spreading. CO2 strongly affects the NaCl-induced atmospheric corrosion rate of copper. The overall influence of CO2 and NaCl depends on at least three identified mechanisms. At low NaCl particle density, CO2 affects the secondary spreading effect from the electrolyte droplet. This leads to a larger effective cathodic area at low CO2 concentration and a higher corrosion rate. The more alkaline surface electrolyte present at low CO2 concentration also affects the formation of corrosion products and the amount of soluble copper chloride. Whereas the presence of larger amounts of soluble chloride tends to increase the corrosion rate, the formation of CuO results in a more protective surface film which decreases the corrosion rate. This effect was observed at higher NaCl particle densities, where the secondary spreading areas overlapped with adjacent NaCl particle clusters. The formation of CuO leads to lower corrosion rates compared to ambient CO2 concentration in which this phase was not formed. For zinc, the formation of a more protective corrosion product layer was not observed and the corrosion rate is generally higher for low than for ambient CO2 concentration. The presence of NaCl particles on the metal surfaces strongly affects the SO2 interaction with the metal surfaces. The oxidation of S(IV) turned out to be fast at the area of the NaCl-containing electrolyte droplet, both for copper and zinc. On copper surfaces, both sulphate (SO4 2-) and dithionate (S2O6 2-) ions formed which is consistent with a copper catalysed reaction route for sulfite oxidation including the formation of a Cu(II)–sulfito complex as an important step. For zinc, a surface mediated sulfite oxidation process leads to rapid formation of sulphate in the electrolyte droplet area. The presence of SO2 strongly inhibits the secondary spreading due to the decrease in pH induced by absorption of SO2 in the cathodic areas. The presence of gaseous oxidants, such as NO2 and O3, has previously been considered as an important prerequisite for the oxidation of sulfite on copper. The results obtained here suggest that the formation of local electrochemical cells induced by deposited NaCl particles could be another important route for S(IV)- oxidation to sulfate formation. On copper, SO2 was also found to promote the formation of less soluble copper chlorides, such as paratacamite (Cu2(OH)3Cl) and nantokite (CuCl). The electrolyte droplet was dried after 24 hours of exposure due to the formation of less soluble paratacamite (Cu2(OH)3Cl) and nantokite (CuCl) and led to a decrease in the corrosion rate. Thus, SO2 alone promotes the corrosion rate of copper, whereas in the presence of NaCl particles the corrosion rate of copper may slow down due to the formation of insoluble copper chloride compounds. The lateral distribution of corrosion products after exposure of NaCl contaminated copper and zinc surfaces to humid air with gaseous pollutants is a result of the formation of local electrochemical cells at the particles and concomitant differences in chemical composition and pH. For (NH4)2SO4 deposited copper and zinc surfaces the corrosion effects increase with the amount of pre-deposited particles and with the exposure time. On copper, the size of the particles affects the corrosion rate, smaller particles resulting in a higher corrosion rate than larger particles at equal amount of deposition. The formation of Cu2O was the dominant corrosion product after exposure longer than 10 days. (NH4)2SO4 particles result in enhanced Cu2O formation on copper due to a reaction sequence involving catalysis by NH3. The corrosion of copper by (NH4)2SO4 particles was much larger than that induced by NaCl particles. However, for zinc, the (NH4)2SO4 particles lead to smaller corrosion effects than those of NaCl particles. For both particles, significant corrosion attack was observed at relative humidity (RH) lower than the deliquescence point of the salts.

  • 2.
    Chen, Zhuo Yuan
    et al.
    Swedish Corrosion Institute.
    Persson, D.
    Swedish Corrosion Institute.
    Leygraf, Christofer
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Corrosion Science.
    In situ studies of the effect of SO2 on the initial NaCl-induced atmospheric corrosion of copper2005In: Journal of the Electrochemical Society, ISSN 0013-4651, E-ISSN 1945-7111, Vol. 152, no 12, p. B526-B533Article in journal (Refereed)
    Abstract [en]

    The initial SO2-induced atmospheric corrosion of copper deposited with NaCl has been examined with Fourier transform infrared microspectroscopy under in situ and ex situ conditions in order to reveal the spatial distribution of reaction products. The oxidation of S(IV) turns out to be fast at the area of the NaCl-containing electrolyte droplet, and both sulfate (SO42-) and dithionate (S2O62-) ions form. A copper-catalyzed reaction route for the sulfite oxidation has been suggested, which includes the formation of a Cu(II)-sulfito complex as an important step. The presence of gaseous oxidants such as NO2 and O-3 has previously been considered as an important prerequisite for the oxidation of sulfite on copper. The results obtained here suggest that the formation of local electrochemical cells induced by deposited NaCl particles could be another important route for S(IV) oxidation to sulfate formation. SO2 was found to promote the formation of less soluble paratacamite [Cu-2(OH)(3)Cl] and nantokite (CuCl), which may slow down the atmospheric corrosion rate of copper.

  • 3.
    Chen, Zhuo Yuan
    et al.
    Swedish Corrosion Institute.
    Persson, D.
    Swedish Corrosion Institute.
    Nazarov, A.
    Swedish Corrosion Institute.
    Zakipour, S.
    Swedish Corrosion Institute.
    Thierry, D.
    Swedish Corrosion Institute.
    Leygraf, Christofer
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Corrosion Science.
    In situ studies of the effect of CO2 on the initial NaCl-induced atmospheric corrosion of copper2005In: Journal of the Electrochemical Society, ISSN 0013-4651, E-ISSN 1945-7111, Vol. 152, no 9, p. B342-B351Article in journal (Refereed)
    Abstract [en]

    The effect of carbon dioxide (CO2) on the NaCl-induced atmospheric corrosion of copper was studied using in situ Fourier transform infrared microspectroscopy, in situ scanning Kelvin probe, and scanning electron microscopy/energy-dispersive analysis by X-ray. The copper surface was contaminated with a single NaCl particle and then exposed to 80 +/- 2% relative humidity clean humidified air with two concentrations of CO2 (< 5 and 350 ppm). After formation of an electrolyte droplet secondary spreading of electrolyte from the peripherical parts of the droplet was observed. The secondary spreading effect, which was much larger at < 5 ppm CO2 than at 350 ppm, was a consequence of the formation of a galvanic element between a local cathode outside the edge of the droplet and an anode in the droplet. This lead to alkaline conditions in the secondary spreading area and transport of Na+ ions to the local cathode. The large secondary spreading at low CO2 concentration was possible due to lowering of the surface tension of the electrolyte/metal oxide interface at the peripheral parts of the droplet. Carbonate formation lowered the pH when the CO2 concentration was 350 ppm and resulted in a decrease of the pH and inhibition of the secondary spreading.

  • 4.
    Chen, Zhuo Yuan
    et al.
    Swedish Corrosion Institute.
    Persson, D.
    Swedish Corrosion Institute.
    Samie, F.
    Swedish Corrosion Institute.
    Zakipour, S.
    Swedish Corrosion Institute.
    Leygraf, Christofer
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Corrosion Science.
    Effect of carbon dioxide on sodium chloride-induced atmospheric corrosion of copper2005In: Journal of the Electrochemical Society, ISSN 0013-4651, E-ISSN 1945-7111, Vol. 152, no 12, p. B502-B511Article in journal (Refereed)
    Abstract [en]

    The effect of carbon dioxide (CO2) on sodium chloride (NaCl) induced atmospheric corrosion of copper was studied in laboratory exposures using microgravimetry, ion chromatography, Fourier transform infrared spectroscopy, and scanning electron microscopy with X-ray microanalysis. With lower amount of NaCl particles on the copper surface (< 15 mu g/cm(2)), the corrosion rate was higher with < 1 ppm CO2 than with 350 ppm CO2, and for higher amount of NaCl (> 15 mu g/cm(2)), the corrosion was higher with 350 ppm CO2. With lower amount of NaCl and low CO2 concentration, a secondary spreading of electrolyte occurred from the droplets that formed at the particle clusters. This led to a larger effective cathodic area and a higher corrosion rate. However, at higher surface concentration of NaCl a spatial interaction effect between the local corrosion sites counteracted the increase in the corrosion rate due to overlap of the cathodic areas from the particles. Another factor, which influenced the corrosion process, was the effect of CO2 on the pH of the surface electrolyte. Higher pH (< 1 ppm CO2 concentration) increased the formation of CuO, which improved the corrosion resistance of the corrosion product layer but hindered the formation of insoluble CuCl, whereby more soluble chloride ions were available for triggering localized corrosion and accelerating the initial atmospheric corrosion of copper. Hence, the overall influence of CO2 and NaCl depends on at least three identified mechanisms.

  • 5. Chen, Zhuo Yuan
    et al.
    Persson, Dan
    Leygraf, Christofer
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Corrosion Science.
    Initial NaCl- Particle Induced Atmospheric Corrosion of Zinc-Effect of CO2 and SO22008In: Corrosion Science, ISSN 0010-938X, E-ISSN 1879-0496, Vol. 50, no 1, p. 111-123Article in journal (Refereed)
    Abstract [en]

    Initial corrosion and secondary spreading effects during NaCl particle induced corrosion on zinc was explored using in situ and ex situ FTIR microspectroscopy, optical microscopy, and SEM/EDAX. The secondary spreading effect which occurs upon introduction of humid air on NaCl deposited zinc surfaces was strongly dependent on the CO2 and SO2 content of the introduced air. Ambient level of CO2 (350 ppm) resulted in a relatively low spreading effect, whereas the lower level of CO2 (<5 ppm) caused a much faster spreading over a larger area. In the presence of SO2, the secondary spreading effect was absent which could limit the cathodic process in this case. At <5 ppm CO2, the corrosion is more localized, with the formation of simonkolleite (Zn5(OH)8Cl2 · H2O), zincite (ZnO) and sodium carbonate (Na2CO3), and a larger effective cathodic area. At 350 ppm CO2, the corrosion is more general and formation of simonkolleite, hydrozincite (Zn5(OH)6(CO3)2) and sodium carbonate was observed. Sodium carbonate was mainly formed in more alkaline areas, in the inner edge of the electrolyte droplet and in the secondary spreading area. Oxidation of sulphur and concomitant sulphate formation was enhanced in the presence of NaCl particles, due to the formation of a droplet, the separation of the anodic and cathodic areas and the accompanying differences in chemical composition and pH in the surface electrolyte.

  • 6.
    Chen, Zhuo Yuan
    et al.
    Swedish Corrosion Institute.
    Tidblad, J.
    Swedish Corrosion Institute.
    Persson, D.
    Swedish Corrosion Institute.
    Zakipour, S.
    Swedish Corrosion Institute.
    Kucera, V.
    Swedish Corrosion Institute.
    Leygraf, Christofer
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Corrosion Science.
    The Effect of Ammonium Sulfate Particles on the Atmospheric Corrosion of CopperManuscript (preprint) (Other academic)
  • 7.
    Chen, Zhuo Yuan
    et al.
    KTH, Superseded Departments, Materials Science and Engineering.
    Zakipour, S.
    Persson, D.
    Leygraf, Christofer
    KTH, Superseded Departments, Materials Science and Engineering.
    The Effect of Sodium Chloride Particles on the Atmospheric Corrosion of Pure Copper2004In: Corrosion, ISSN 0010-9312, E-ISSN 1938-159X, Vol. 60, no 5, p. 479-491Article in journal (Refereed)
    Abstract [en]

    The atmospheric corrosion of copper has been investigated after deposition of sodium chloride (NaCl) particles and 10 days of subsequent exposure to clean, humidified air below, near, and above the point of deliquescence of NaCl (at around 75% relative humidity (RH), Microgravimetry, Fourier transform infrared (FTIR) microspectroscopy, scanning electron microscopy with x-ray microanalysis, and scanning Kelvin probe were used to identify corrosion processes and products. The NaCl deposition resulted in the evenly distributed NaCl particle clusters with a diameter of approximately 100 μm. The clusters consisted of individual NaCl particles of <10 μm. The mass gain increased linearly with the amount of NaCl particles added in the range of this study (up to 4 μg/cm2). Even at very low RH (55%), which lies far below the point of deliquescence (75%), copper with NaCl particles added suffered from significant corrosion attack and the mass gain of copper with 4 μg/cm2 NaCl added was about 7 μg/cm2 after 10 days of exposure. At 55% RH, the NaCl particles did not dissolve. However, significant chloride-induced corrosion effects were observed after 10 days, both in the original particle cluster and in a 20-μm-wide outer zone into which chloride ions had dffused radially. At 75% RH, the NaCl particles dissolved and chloride ions diffused to cover the whole surface. Chloride-accelerated corrosion effects resulted in the formation of cuprite (Cu2O) and copper carbonate, mainly in the area of the original particle cluster. The corrosion effects accelerated further at 95% PH, resulting in the formation of Cu2O over the whole surface and copper carbonate in a concentric zone outside the original particle cluster. The distribution of the corrosion products was related to the localization of the anodic and cathodic reactions during the corrosion process.

  • 8.
    Chen, Zhuo Yuan
    et al.
    wedish Corrosion Institute, Sweden.
    Zakipur, S.
    Persson, D.
    Leygraf, Christofer
    KTH, School of Chemical Science and Engineering (CHE), Chemistry, Corrosion Science (closed 20081231).
    The Combined Effects of Gaseous pollutants and Sodium Chloride Particles on the Atmospheric Corrosion of Pure Copper2005In: Corrosion, ISSN 0010-9312, E-ISSN 1938-159X, Vol. 61, no 11, p. 1022-1034Article in journal (Refereed)
    Abstract [en]

    The atmospheric corrosion of pure copper has been investigated after the deposition of sodium chloride (NaCI) particles and exposure to humid air containing gaseous pollutants. Microgravimetry, Fourier transform infrared (FTIR) micro-spectroscopy, and scanning electron microscopy with x-ray microanalysis were used for the investigation of corrosion processes and products. The effect of NaCl particles on the mass gain was much higher than that of gaseous pollutants. With deposition of NaCl particles on the copper surfaces, the corrosion rate increased significantly, with severe corrosion attack mainly localized to the NaCl particle clusters. A similar corrosion rate was found, however, after exposure to pure humid air and to humid air containing gaseous pollutants, sulfur dioxide (SO2), ozone (O-3), nitrogen dioxide (NO2), and SO2 + NO2. The corrosion rate was not dependent on the concentration of the pollutants. However, this was not the case for the combination of SO2 and O-3, leading to a significantly higher corrosion rate at higher concentrations. Exposure of copper samples with NaCl particles deposited resulted in unevenly distributed corrosion product clusters, with a distribution of corrosion products that could be associated with the locations of the particle clusters. Around the particle clusters, the corrosion resulted in areas with different amounts of corrosion products. After 10 days of exposure to humid air containing 100 ppb SO2 and 100 ppb NO2 + SO2, cuprite (Cu2O), paratacamite (Cu-2[OH](3)Cl), carbonate (CO32-), and sulfate (SO42-) were observed mainly in the area of the original particle cluster, with some sutfate and copper hydroxysulfate also in the areas outside. After 10 days of exposure to humid air containing 100 ppb O-3 + SO2, cuprite (Cu2O), hydroxychloride (maybe paratacamite, Cu-2[OH](3)Cl), carbonate (CO32-), and sutfate (SO42-) were observed in the area of the original particle cluster. A circular zone containing brochantite (Cu-4[OH](6)SO4) was formed around and outside of the original particle cluster, and the formation of this phase was promoted by the presence of NaCl particles on the surface. The location of anodic and cathodic reactions during the corrosion process leads to the distribution of different corrosion products on the surface.

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