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Materials and Design 87 (2015) 266–271

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Materials and Design

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Study of influence of gamma prime and eta phases on corrosion behaviour
of A286 superalloy by using electrochemical potentiokinetic techniques
Óscar Martín a,⁎, Pilar De Tiedra b, Manuel San-Juan a
a
Ingeniería de los Procesos de Fabricación, Departamento CMeIM/EGI/ICGF/IM/IPF, Universidad de Valladolid, Escuela de Ingenierías Industriales, Paseo del Cauce 59, Valladolid 47011, Spain
b
Ciencia de los Materiales e Ingeniería Metalúrgica, Departamento CMeIM/EGI/ICGF/IM/IPF, Universidad de Valladolid, Escuela de Ingenierías Industriales, Paseo del Cauce 59, Valladolid 47011, Spain

a r t i c l e i n f o a b s t r a c t

Article history: This work studies the influence of gamma prime and eta phases, resulting from precipitation hardening, on the
Received 1 June 2015 corrosion behaviour of A286 superalloy by using electrochemical potentiokinetic reactivation (EPR) and double
Received in revised form 23 July 2015 loop electrochemical potentiokinetic reactivation (DLEPR). The general trend is that Ir, Qr, Ir/Ia and Qr/Qa increase
Accepted 9 August 2015
with aging temperature and, for a given aging temperature, with aging time, which is consistent with the fact that
Available online 14 August 2015
gamma prime precipitate may cause discontinuities in the passive layer. Ir, Qr, Ir/Ia and Qr/Qa reach a peak, which
Keywords:
alters the general trend, for both aging temperatures (670 and 720 °C), at the aging time from which there is
A286 superalloy evidence of the presence of eta phase at grain boundary (GB). Gamma prime and eta precipitates can cause
Precipitation hardening the passive layer that forms on them to become more unstable and, consequently, cause the current density
EPR through the passive layer and the susceptibility to localized corrosion attack to increase.
DLEPR © 2015 Elsevier Ltd. All rights reserved.
SEM

1. Introduction the hydrogen embrittlement sensitivity because the η phase/matrix in-
terface is incoherent and, consequently, more prone to accumulate hy-
A286 superalloy is a precipitation-hardenable austenitic stainless drogen during the plastic deformation, which enhances de-cohesion
steel which is widely used in gas turbine industry as gas turbine and, hence, leads to fracture; and, Rho et al. [13] pointed out
transition-piece material, which connects the gas turbine to the power that, since provides the site for the GB cavitation which promotes
turbine inlet, due to its good thermal resistance, superior mechanical the intergranular failures, induces the decrease in fatigue life.
properties, and ease of fabrication [1]; it is also utilized, as indicated Conversely, Li et al. [8] showed that the cellular η phase improves the
by Savoie et al. [2], for reactor vessel internal bolting applications high temperature ductility because its precipitation at GBs causes the
in the nuclear industry because its thermal coefficient of expansion is replacement of primary relatively smooth GBs by new jagged GBs,
comparable to that of AISI 304 stainless steel. which can restrain GB sliding and cracking during high temperature
A286 superalloy is strengthened by the precipitation of the ordered deformation.
fcc gamma prime (γ′) Ni3(Al,Ti) phase [3,4], which is coherent with While the mechanism of precipitation strengthening has been
the matrix [5,6]. Since, according to Seifollahi et al. [7], the γ′ phase widely studied, the influence of γ′ and η phases on corrosion behaviour
is unstable, after a sufficiently long aging treatment at sufficiently of A286 has been much less studied.
high temperature and dissolves to form the hcp eta (η) Ni3Ti phase. Li The present work aims to study the influence of γ′ and η phases
et al. [8] indicated that, at aging temperatures in the range of 600– formed during the precipitation hardening process on the corrosion
850 °C, the η phase precipitates at grain boundary (GB) by cellular behaviour of A286 superalloy.
reaction [9]. Electrochemical potentiokinetic reactivation (EPR) and double
The cellular η phase precipitation at GBs may be detrimental to the loop electrochemical potentiokinetic reactivation (DLEPR) are quasi
mechanical properties as evidenced by several authors: De Cicco et al. non-destructive tests which are much quicker, more sensitive and
[10] showed that degrades the creep behaviour; Brooks and Thompson more accurate than the conventional corrosion tests and that
[11] demonstrated that gives rise to the increase in intergranular have been primarily used to assess the degree of sensitization in
fracture in the tensile test; Guo et al. [12] reported that aggravates austenitic stainless steels [14,15]; nevertheless, as pointed out by
Prohaska et al. [16], they can also provide information on the general
corrosion behaviour and how this may be affected by microstructural
changes. Therefore, EPR and DLEPR techniques were used to assess the
⁎ Corresponding author. effect of γ′ and η phases on the current density through the passive
E-mail address: oml@eii.uva.es (Ó. Martín). layer.

http://dx.doi.org/10.1016/j.matdes.2015.08.041
0264-1275/© 2015 Elsevier Ltd. All rights reserved.
Ó. Martín et al. / Materials and Design 87 (2015) 266–271 267

Table 1
Chemical composition of A286 superalloy (wt.%).

C Si Mn P S Cr Mo Ni V Ti Al B

0.032 0.50 1.24 0.011 b0.0003 14.98 1.18 24.74 0.29 2.30 0.16 0.0046

2. Experimental procedure [20], an electrochemical conditioning was performed. The electrolyte
was 0.5 M H2SO4 + 0.01 M KSCN and the test temperature was
2.1. Materials 30 °C ± 1. The experimental procedure was the following: a delay of
5 min at open circuit (OC) potential, deaerated, an anodic attack at
The chemical composition of A286 superalloy is shown in Table 1. The −220 mV(SCE) for 2 min, a delay of 2 min at VOC, a cathodic cleaning
as-received material was in sheet form whose thickness was 2.2 mm. at − 600 mV(SCE) for 1 min and a delay of 5 min at VOC. Passivation
was accomplished by applying 200 mV(SCE) for 2 min. The reactivation
2.2. Precipitation hardening process scan started at 200 mV until 50 mV below VOC at a rate of 100 mV/min.
The EPR parameters Ir (maximum reactivation current density) and
There were 16 different precipitation hardening conditions which Qr (reactivation charge), were used to assess the corrosion behaviour
were obtained by the processes detailed in Table 2. and are shown in Fig. 1.

2.3. Tensile tests
2.5.2. DLEPR test performance
The tensile test was conducted, for each of the 16 precipitation DLEPR test was carried out according to conditions used in previous
hardening conditions and also for the solution treatment condition, at works [15,20]. The electrolyte was 0.5 M H2SO4 + 0.01 M KSCN
a crosshead speed of 2 mm/min and at room temperature, according [21] and the test temperature was 30 °C ± 1. The three stages of
to ISO 6892-1:2009 [17]. The test piece used was flat with an original the test were: (i) a 5 min delay at VOC; (ii) an anodic polarization
thickness (a0) of 2.2 mm, a parallel length (Lc) of 60 mm and an original scan from 50 mV below VOC to 300 mV(SCE) in the passive range at a
width of the parallel length (b0) of 12.5 mm. scan rate of 100 mV/min; and (iii) a cathodic reactivation scan from
300 mV(SCE) to 50 mV below VOC at the same scan rate.
2.4. Scanning Electron Microscope (SEM) The ratio between maximum reactivation current density during
reverse scan (Ir) and maximum activation current density during anodic
SEM micrographs were obtained after mechanical polishing and scan (Ia), Ir/Ia (%), and the ratio between charges in the reactivation scan
electrolytic etching with etchant No. 83 according to ASTM E407-07e1 (Qr) and in the activation scan (Qa), Qr/Qa (%), were used to evaluate the
(at 6 V for 60 s in a solution of 10 g CrO3 in 100 ml water) [18]. corrosion behaviour.

2.5. EPR and DLEPR tests
3. Results and discussion
EPR and DLEPR tests were performed, for each of the 16 precipitation
hardening conditions and also for the solution treatment condition, by The much higher yield strengths achieved by each of the 16
using a large-scale electrochemical cell which had two high-purity precipitation hardening conditions compared to that achieved by the
carbon auxiliary (counter) electrodes and a saturated calomel electrode solution treatment condition (Fig. 2) are indicative of the strengthening
(SCE) positioned in front of the specimen at a distance of 4 mm. γ′ phase precipitation. According to Thompson and Brooks [4], γ′ phase
is precipitated early in aging and subsequent aging is basically a coars-
2.5.1. EPR test performance ening process where strength increases with increasing γ′ precipitate
EPR test was conducted following ASTM Standard G108-92 [19] but, size until a maximum strength is reached [22–24]; hence, the results
since the results may be dependent on the degree of surface preparation of tensile tests are consistent with [4,22] and also with that of

Table 2
Each of the 16 precipitation hardening conditions consisted of the solution treatment
condition followed by one of the 16 aging conditions.

Solution treatment condition Aging conditions

Temperature (°C) Time (h) Temperature (°C) Time (h)

927 0.25 670 0.5
5
10
25
50
100
150
200
720 0.5
5
10
25
Fig. 1. EPR curves of: (A) solution treatment condition; (B) solution treatment followed by
50
aging treatment at 670 °C for 150 h; (C) solution treatment followed by aging treatment at
100
670 °C for 50 h; and (D) solution treatment followed by aging treatment at 670 °C for
150
100 h, in this curve Ir (maximum reactivation current density, (Ir)D) and Qr (reactivation
200
charge, area under D1–D2–D3) are shown.
268 Ó. Martín et al. / Materials and Design 87 (2015) 266–271

Fig. 2. Yield strength (0.2% offset), obtained from each of the 16 precipitation hardening
conditions, as a function of aging time and aging temperature. The yield strength (0.2% Fig. 5. DLEPR curves of: (A) Solution treatment condition; (B) solution treatment followed
offset) obtained from solution treatment (ST) condition (aging time equal to 0 h) is also by aging treatment at 720 °C for 5 h; (C) solution treatment followed by aging treatment at
provided as a reference value. 720 °C for 50 h; (D) solution treatment followed by aging treatment at 720 °C for 25 h.

Fig. 6. Ratio between maximum reactivation current density during reverse scan (Ir) and
Fig. 3. Maximum reactivation current density, Ir (A/cm2), obtained from the EPR test
maximum activation current density during anodic scan (Ia), Ir/Ia (%), obtained from the
performed for each of the 16 precipitation hardening conditions and also for the solution
DLEPR test performed for each of the 16 precipitation hardening conditions and also for
treatment (ST) condition (aging time equal to 0 h). The EPR tests performed for the
the solution treatment (ST) condition (aging time equal to 0 h). The DLEPR tests
precipitation hardening conditions for which Ir reaches a peak were repeated four
performed for the precipitation hardening conditions for which Ir/Ia reaches a peak were
times; the value shown is the mean value and the error bar is the standard deviation of
repeated four times; the value shown is the mean value and the error bar is the standard
the four repeated tests.
deviation of the four repeated tests.

Zhao et al. [25], which demonstrated that the growth kinetics of γ′ DLEPR curves (Fig. 5) were analysed by using Ir/Ia (Fig. 6) and Qr/Qa
precipitates is faster at higher aging temperatures. (Fig. 7) parameters; the greater the value of Ir, Qr, Ir/Ia or Qr/Qa, the
The results obtained from EPR curves (Fig. 1) were analysed by using higher the current density through the passive layer and, consequently,
Ir (Fig. 3) and Qr (Fig. 4) parameters, and the results obtained from

Fig. 7. Ratio between charges in the reactivation scan (Qr) and in the activation scan (Qa),
Fig. 4. Reactivation charge, Qr (C/cm2), obtained from the EPR test performed for each of the Qr/Qa (%), obtained from the DLEPR test performed for each of the 16 precipitation
16 precipitation hardening conditions and also for the solution treatment (ST) condition hardening conditions and also for the solution treatment (ST) condition (aging time
(aging time equal to 0 h). The EPR tests performed for the precipitation hardening equal to 0 h). The DLEPR tests performed for the precipitation hardening conditions for
conditions for which Qr reaches a peak were repeated four times; the value shown is the which Qr/Qa reaches a peak were repeated four times; the value shown is the mean
mean value and the error bar is the standard deviation of the four repeated tests. value and the error bar is the standard deviation of the four repeated tests.
Ó. Martín et al. / Materials and Design 87 (2015) 266–271 269

Fig. 8. SEM micrographs of A286 superalloy subjected to solution treatment followed by (A) aging treatment at 720 °C for 10 h, there is no cellular η phase; and by (B) aging treatment at
720 °C for 25 h, presence of cellular η phase at GB. Electrolytic etching with etchant No. 83 according to ASTM E407-07 [18].

Fig. 9. SEM micrographs of A286 superalloy subjected to solution treatment followed by (A) aging treatment at 670 °C for 50 h, there is no cellular η phase; and by (B) aging treatment at
670 °C for 100 h, presence of cellular η phase, whose lamellar structure is shown in detail, at GB. Electrolytic etching with etchant No. 83 according to ASTM E407-07 [18].

the greater the susceptibility to localized corrosion attack. With the aim for which Ir/Ia and Qr/Qa parameters reach a peak were repeated
of verifying the reproducibility of the results, the EPR tests performed (three more times on the same sample after the original test, i.e., four
for the precipitation hardening conditions for which Ir and Qr parame- times).
ters reach a peak were repeated (three more times on the same sample As it is shown in Figs. 3 and 4, the general trend is that both Ir and Qr
after the original test, i.e., four times); and in the same manner increase with increasing aging time, but this trend is altered by a peak
the DLEPR tests performed for the precipitation hardening conditions that, for the aging temperatures of 720 °C and 670 °C, is reached at an

Fig. 10. SEM micrographs of A286 superalloy subjected to solution treatment followed by (A) aging treatment at 720 °C for 25 h, no sign of intragranular localized corrosion attack can be
appreciated; and by (B) aging treatment at 720 °C for 200 h, the arrows show the intragranular localized corrosion attack. The micrographs were taken after EPR test.
270 Ó. Martín et al. / Materials and Design 87 (2015) 266–271

Fig. 11. SEM micrograph of A286 superalloy subjected to solution treatment followed Fig. 13. EDX line scan (wt.%) for Cr and Ni across the GB. SEM micrograph of A286 super-
by aging treatment at 670 °C for 200 h. The figure shows the γ′ and η phases and the alloy subjected to solution treatment followed by aging treatment at 670 °C for 200 h. The
γ′-free zones surrounding η phase. Electrolytic etching with etchant No. 83 according to micrograph was taken after EPR test.
ASTM E407-07 [18].

aging time of, respectively, 25 h and 100 h. The results obtained from consistent with the fact that, as pointed out by Číhal and Štefec [26],
DLEPR (Figs. 6 and 7) are consistent with that from EPR and, hence, γ′ precipitate distributed throughout the matrix may cause discontinu-
the general trend is also that Ir/Ia and Qr/Qa increase with increasing ities in the passive layer.
aging time, but this trend is altered by a peak that, for an aging temper- The effect of η phase on the corrosion behaviour and its relation to
ature of 720 °C, is reached at an aging time of 25 h and, for an aging the peak shown in Figs. 3, 4, 6 and 7 may be explained by (i) the fact
temperature of 670 °C, at an aging time of 100 h. At 720 °C, 25 h is that η phase grows at the expense of γ′ phase [27,28] and consequently
the aging time from which there is evidence of the presence of η γ′-free zones surrounding η phase (Fig. 11), as demonstrated by
phase (Fig. 8) and at 670 °C, 100 h is the aging time from which there Seifollahi et al. [7] and by Zhao et al. [29]; and (ii) by a post-EPR
is evidence of the presence of η phase (Fig. 9). microstructural study that shows a localized corrosion attack at GB
Therefore, Ir, Qr, Ir/Ia and Qr/Qa reach a peak, for both aging tempera- which becomes more extensive and continuous as the aging time
tures (670 and 720 °C), at the aging time from which there is evidence of increases (Fig. 12), this localized corrosion attack at GB, as it is shown
the presence of η phase at GB. in Fig. 13, is not associated with chromium depletion but with the
The effect of γ′ precipitates on the corrosion behaviour, which is precipitation of the nickel-rich η phase at GB (its surrounding area is
shown is Figs. 3, 4, 6 and 7, was verified by a post-EPR microstructural nickel-depleted).
study which shows a localized corrosion attack homogeneously distrib- The results obtained from EPR are consistent with that from DLEPR,
uted into the grain which becomes more extensive as γ′ precipitates but EPR allows a better appreciation of the differences between suscep-
grow, i.e., as the aging time increases (Fig. 10). tibilities to corrosion attack at different aging temperatures; this result
Therefore, the increase of Ir, Qr, Ir/Ia and Qr/Qa with aging tempera- confirms that the sensitivity of EPR is greater than that of DLEPR at
ture and, for a given aging temperature, with aging time (Fig. 10) is lower intensities of corrosion attack [30].

Fig. 12. SEM micrographs of A286 superalloy subjected to solution treatment followed by (A) aging treatment at 720 °C for 25 h; and by (B) aging treatment at 720 °C for 200 h. The figure
shows the localized corrosion attack at GB (more extensive and continuous in (B) than in (A)). The micrograph was taken after EPR test.
Ó. Martín et al. / Materials and Design 87 (2015) 266–271 271

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