• Proceedings of the KWS Conference
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• 2002.10a
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• pp.250-254
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• 2002

Intergranular corrosion of austenitic stainless steels is a conventional and momentous problem during welding and high temperature use. One of the major reasons for such intergranular corrosion is so-called sensitization, i.e., chromium depletion due to chromium carbide precipitation at grain boundaries. Conventional methods for preventing sensitization of austenitic stainless steels include reduction of carbon content in the material, stabilization of carbon atoms as non-chromium carbides by the addition of titanium, niobium or zirconium, local solution-heat-treatment by laser beam, etc. These methods, however, are not without drawbacks. Recent grain boundary structure studies have demonstrated that grain boundary phenomena strongly depend on the crystallographic nature and atomic structure of the grain boundary, and that grain boundaries with coincidence site lattices are immune to intergranular corrosion. The concept of "grain boundary design and control", which involves a desirable grain boundary character distribution, has been developed as grain boundary engineering. The feasibility of grain boundary engineering has been demonstrated mainly by thermomechanical treatments. In the present study, a thermomechanical treatment was tried to improve the resistance to the sensitization by grain boundary engineering. A type 304 austenitic stainless steel was pre-strained and heat-treated, and then sensitized, varying the parameters (pre-strain, temperature, time, etc.) during the thermomechanical treatment. The grain boundary character distribution was examined by orientation imaging microscopy. The intergranular corrosion resistance was evaluated by electrochemical potentiokinetic reactivation and ferric sulfate-sulfuric acid tests. The sensitivity to intergranular corrosion was reduced by the thermomechanical treatment and indicated a minimum at a small roll-reduction. The frequency of coincidence-site-lattice boundaries indicated a maximum at a small strain. The ferric sulfate-sulfuric acid test showed much smaller corrosion rate in the thermomechanically-treated specimen than in the base material. An excellent intergranular corrosion resistance was obtained by a small strain annealing at a relatively low temperature for long time. The optimum parameters created a uniform distribution of a high frequency of coincidence site lattice boundaries in the specimen where corrosive random boundaries were isolated. The results suggest that the thermomechanical treatment can introduce low energy segments in the grain boundary network by annealing twins and can arrest the percolation of intergranular corrosion from the surface.

• Nuclear Engineering and Technology
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• v.50 no.7
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• pp.1131-1137
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• 2018

The effect of a serrated grain boundary on stress corrosion cracking (SCC) of Alloy 600 was investigated in terms of improvement of SCC resistance. Serrated grain boundaries and straight grain boundaries were obtained by controlled heat treatment. SCC cracks preferentially initiated and grew at grain boundaries normal to the tensile loading axis. Resolved tensile stress normal to the grain boundary was lower in serrated grain boundaries compared to straight grain boundaries. The specimen with serrated grain boundaries showed higher SCC resistance than that with straight grain boundaries due to a lower resolved tensile stress normal to the grain boundary.

• Corrosion Science and Technology
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• v.14 no.6
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• pp.313-324
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• 2015

Austenitic stainless steels have been widely used in many engineering fields because of their high corrosion resistance and good mechanical properties. However, welding or aging treatment may induce intergranular corrosion, stress corrosion cracking, pitting, etc. Since these types of corrosion are closely related to the formation of chromium carbide in grain boundaries, the alloys are controlled using methods such as lowering the carbon content, solution heat treatment, alloying of stabilization elements, and grain boundary engineering. This work focused on the effects of aging and UNSM (Ultrasonic Nano-crystal Surface Modification) on the intergranular corrosion of commercial 316L stainless steel and the results are discussed on the basis of the sensitization by chromium carbide formation and carbon segregation, residual stress, grain refinement, and grain boundary engineering.

• Corrosion Science and Technology
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• v.2 no.2
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• pp.82-87
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• 2003

Stress corrosion cracking of Alloy 600 and Alloy 690 has been studied with a C-ring specimen in 1%, 10% and 40% NaOH at $315^{\circ}C$. SCC test was performed at 200 mV above corrosion potential. Initial stress on the apex of C-ring specimen was varied from 300 MPa to 565 MPa. Materials were heat treated at various temperatures. SCC resistance of Ni-$_\chi$Cr-10Fe alloy increased as the Cr content of the alloy increased if the density of an intergranular carbide were comparable. SCC resistance of Alloy 600 increased in caustic solution as the product of coverage of an intergranular carbide in grain boundary, intergranular carbide thickness and Cr concentration at grain boundary increased. Low temperature mill annealed Alloy 600 with small grain size and without intergranular carbide was most susceptible to SCC. TT Alloy 690 was most resistant to SCC due to the high value of the product of coverage of an intergranular carbide in grain boundary, intergranular carbide thickness and Cr concentration at grain boundary. Dependency of SCC rate on stress and NaOH concentration was obtained.

• Corrosion Science and Technology
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• v.12 no.6
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• pp.265-273
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• 2013

Ti-stabilized 11 wt% Cr ferritic stainless steels (FSSs) for automotive exhaust systems have been experienced intergranular corrosion (IC) in some heat-affected zone (HAZ). The effects of sensitizing heat-treatment and silicon on IC were studied. Time-Temperature-Sensitization (TTS) curves showed that sensitization to IC was observed at the steels heat-treated at the temperature lower than $650^{\circ}C$ and that silicon improved IC resistance. The sensitization was explained by chromium depletion theory, where chromium is depleted by precipitation of chromium carbide during sensitizing heat-treatment. It was confirmed with the results from the analysis of precipitates as well as the thermodynamical prediction of stable phases. In addition, the role of silicon on IC was explained with the stabilization of grain boundary. In other words, silicon promoted the formation of the grain boundaries with low energy where precipitation was suppressed and consequently, the formation of Cr-depleted zone was retarded. The effect of silicon on the formation of grain boundaries with low energy was proved by the analysis of coincidence site lattice (CSL) grain boundary, which is a typical grain boundary with low energy.

• ETRI Journal
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• v.21 no.3
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• pp.16-21
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• 1999

After etching Al-Cu alloy films using SiCl4/Cl_2/He/CHF3 mixed gas plasma, the corrosion phenomenon at the grain boundary of the etched surface and a passivation layer on the etched surface with an SF6 plasma treatment subsequent to the etching were studied. In Al-Cu alloy system, corrosion occurs rapidly on the etched surface by residual chlorine atoms, and it occurs dominantly at the grain boundaries rather than the crystalline surfaces. To prevent corrosion, the SF6 gas plasma treatment subsequent to etching was carried out. The passivation layer is composed of fluorine-related compounds on the etched Al-Cu surface after the SF6 treatment, and it suppresses effectively corrosion on the surface as the SF6 treatment pressure increases. Corrosion could be suppressed successfully with the SF6 treatment at a total pressure of 300 mTorr. To investigate the reason why corrosion could be suppressed with the SF6 treatment, behaviors of chlorine and fluorine were studied by various analysis techniques. It was also found that the residual chlorine incorporated at the grain boundary of the etched surface accelerated corrosion and could not be removed after the SF6 plasma treatment.

• Corrosion Science and Technology
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• v.6 no.4
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• pp.170-176
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• 2007

Iodine-induced stress corrosion cracking (ISCC) properties and the associated ISCC process of Zircaloy-4 and an Nb-containing advanced nuclear fuel cladding were evaluated. An internal pressurization test with a pre-cracked specimen was performed with a stress-relieved (SR) or recrystallized (RX) microstructure at $350^{\circ}C$, in an iodine environment. The results showed that the $K_{ISCC}$ of the SR and RX Zircaloy-4 claddings were 3.3 and 4.8MPa\;m^{0.5}, respectively. And the crack propagation rate of the RX Zircaloy-4 was 10 times lower than that of the SR one. The chemical effect of iodine on the crack propagation rate was very high, which was increased $10^4$ times by iodine addition. Main factor affecting on the micro-crack nucleation was a pitting formation and its agglomeration along the grain boundary. However, this pitting formation on the grain-boundary was suppressed in the case of an Nb addition, which resulted in an increase of the ISCC resistance when compared to Zircaloy-4. Crack initiation and propagation mechanisms of fuel claddings were proposed by a grain boundary pitting model and a pitting assisted slip cleavage model and they showed reasonable results.

• Corrosion Science and Technology
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• v.11 no.4
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• pp.141-150
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• 2012

Stress corrosion cracks in Alloy 600 compact tension specimens tested at $325^{\circ}C$ in a simulated primary water environment of pressurized water reactor were analyzed by analytical transmission electron microscopy and secondary ion mass spectroscopy (SIMS). From a fine-probe chemical analysis, oxygen was found on the grain boundary just ahead of the crack tip, and chromium oxides were precipitated on the crack tip and the grain boundary attacked by the oxygen diffusion, leaving a Cr/Fe depletion (or Ni enrichment) zone. The oxide layer inside the crack was revealed to consist of a double (inner and outer) layer. Chromium oxides existed in the inner layer, with NiO and (Ni,Cr) spinels in the outer layer. From the nano-SIMS analysis, oxygen was detected at the locations of intergranular chromium carbides ahead of the crack tip, which means that oxygen diffused into the grain boundary and oxidized the surfaces of the chromium carbides. The intergranular chromium carbide blunted the crack tip, thereby suppressing the crack propagation.

• Journal of the Korean Institute of Telematics and Electronics A
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• v.33A no.12
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• pp.47-52
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• 1996

Cl-based gas chemistry is generally used to etching for al alloy metallization. After the etching of Al alloy with Cl-based gas plasma, residual chlorine on Al alloy reacts with H$_{2}$O due to air exposure and results in Al corrosion. In this study, the corrosion phenomena of Al wer examined with XPS(X-ray photoelectron spectroscopy) and SEM (scanning electorn microscopy). It was confirmed that chlorine mainly existed at the grian boundary of Al alloy after plasma etching of Al alloy with cl-based gas chemistry and Al corrosion was largely generated at the grain boundary of Al alloy. And residual chlorine was passivated by sulfur and fluorine which were generated by SF$_{6}$ plasma. These effects of passivation reduced the Al corrosion due to air exposure.

• Korean Journal of Materials Research
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• v.27 no.8
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• pp.431-437
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• 2017

This study investigated the surface pit corrosion of SS420J2 stainless steel accompanied by intergranular crack. To reveal the causes of surface pits and cracks, OM, SEM, and TEM analyses of the microstructures of the utilized SS420J2 were performed, as was simulated heat treatment. The intergranular cracks were found to have been induced by a grain boundary carbide of $(Cr,Fe)_{23}C_6$, which was identified by SEM/EDS and TEM diffraction analyses. The mechanism of grain boundary sensitization occurred at the position of the carbide, followed by its occurrence at the Cr depleted zone. The grain boundary carbide of $(Cr,Fe)_{23}C_6$ type precipitated during air cooling condition after a $1038^{\circ}C$ solid solution treatment. The carbide precipitate formation also accelerated at the band structure formed by cold working. Therefore, using manufacturing processes of cooling and cold working, it is difficult to protect SS420J2 stainless steel against surface pit corrosion. Several counter plans to fight pit corrosion by sensitization were suggested, involving alloying and manufacturing processes.