Linear sweep voltammetry (LSV) test parameters in alkaline medium were optimized by Doehlert matrix design in order to quantify the deleterious phases in a superduplex stainless steel UNS S32750. The microstructural analysis was performed, in several heat treated specimens, by Light Optical (LOM) and Scanning Electron (SEM) Microscopies and correlated with the electrochemical tests. In these tests, optimized parameters were obtained for tests in aqueous solutions of KOH. The concentration of 3.55 mol l −1 , scan rate of 3.42 mV s −1 and initial potential of −0.818 V, showed a good correlation between the deleterious phases precipitated and charge density values. Differently from LOM characterization, chi and sigma deleterious phases can be distinguished by LSV optimized test. Finally, this test can be a non-destructive powerful tool of quality control to detect embrittlement and corrosion resistance decay that commonly affected this stainless steel as consequence of inadequate fabrication processes.

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An optimised electrochemical technique, linear sweep voltammetry (LSV) in KOH solution (LSV-KOH) was confronted with the double loop electrochemical Potentiokinetic reactivation (DL-EPR) to verify which is the best technique to quantify deleterious phases (DP) in a UNS S32750 super duplex stainless steel. DL-EPR presented an error in determination of deleterious phases in the range of 6.9-100%. LSV-KOH show a better accuracy in quantification of deleterious phases volume fractions, the error range for LSV-KOH was 2.4-26.2%. When the morphology of sigma changes from lamellar to divorced, was observed modifications on LSV-KOH voltammograms. In specimens where lamellar morphology is present, the voltammograms show two peaks curve. Meanwhile, in specimens where occurred also divorced precipitation of sigma the voltammograms changes to a 3 peaks curve. This feature is due to the dissolution of sigma phase boundaries which has different compositions according to the form of sigma precipitation.

The corrosion behavior of a 17Cr multiphase martensitic stainless steel quenched (1000°C, water cooling) and tempered at different temperatures was determined using the double-loop electrochemical potentiokinetic reactivation (DL-EPR) test. The specimen tempered at 550°C showed the highest degree of sensitization. For the specimen treated at 600°C, a healing process was observed, followed by a second sensitization at 625°C coincident with an increase in the austenite volume fraction. This phase was quantified using the magnetic method and an increase in this phase was observed with the tempering temperature. The DL-EPR results were correlated with surface aspects obtained by atomic force microscopy.