Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950, doi: 10.20964/2022.09.

49

International Journal of
ELECTROCHEMICAL
SCIENCE
www.electrochemsci.org

Frequency-Time Domain Analysis of Electrochemical Noise of

Passivated AM350 Stainless Steel for Aeronautical Applications
C. Gaona Tiburcio1, O. Samaniego-Gámez1, J.M. Jáquez-Muñoz1,2*, M.A. Baltazar-Zamora2, L. Landa-
Ruiz2, A. Lira-Martínez3, J.P. Flores-De los Rios4, J. Cabral-Miramontes1, F. Estupinán-López1, F.
Almeraya-Calderon1*
1
Universidad Autónoma de Nuevo León, Facultad de Ingeniería Mecánica y Eléctrica, Centro de
Investigación e Innovación en Ingeniería Aeronáutica (CIIIA), Av. Universidad s/n, Ciudad
Universitaria, San Nicolás de los Garza, Nuevo León 66455, México
2
Facultad de Ingeniería Civil-Xalapa, Universidad Veracruzana, Lomas del Estadio S/N, Zona
Universitaria, 91000 Xalapa, Veracruz, Mexico
3
Universidad Autónoma de Ciudad Juárez, Instituto de Ingeniería y Tecnología (IIT), Av. Del Charro
150 N, Ciudad Juárez Chihuahua 32584, Mexico.
4
Department Metal-Mechanical, Tecnológico Nacional de Mexico-Instituto Tecnológico de Chihuahua,
Av. Tecnologico 2909, Chihuahua 31130, Mexico
*
E-mail: [email protected]; [email protected]

Received: 2 June 2022 / Accepted: 19 July 2022 / Published: 7 August 2022

Precipitation-hardening stainless steel is frequently utilized in a variety of aerospace applications. While

the latter steel is employed in applications demanding great strength and corrosion resistance, the former
steel offers good corrosion resistance with moderate strength. In this work, the corrosion behavior of
AM 350 stainless steel exposed to solutions containing 5% NaCl and 1% H2SO4 after being passivated
in nitric acid and citric acid solution for 50 min each at 49 and 70°C is examined. AM 350 stainless steel
is precipitation hardening stainless steel, widely used in various aerospace applications. The former steel
exhibits excellent corrosion resistance with moderate strength, whereas the latter is used for applications
requiring high strength and corrosion resistance. In this study, AM 350 stainless steel corrosion behavior
passivated in a) citric acid and b) nitric acid solutions for 50 min at 49 and 70 °C, and subsequently
exposed in 5 wt. % NaCl and 1 wt. % H2SO4 solutions are investigated. The electrochemical technique
used was electrochemical noise (EN), based on the ASTMG199 standards. Two data analysis techniques
were employed for EN: the time-frequency domain (wavelets transform) and the power spectral density
(PSD). The results showed a better behavior against corrosion of samples passivated in nitric acid in
citric acid. Also, in NaCl electrolyte, the uniform process is the predominant behavior.

Keywords: stainless steel, electrochemical noise, passivation, FFT, Wavelets.

Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 2

1. INTRODUCTION
One of the biggest problems in the aeronautic industry is the corrosion of aircraft components,
increasing costs, and decreasing safety. Nowadays, the methods to protect materials against corrosion
seek to decrease the environmental impact by reducing the contamination of some processes as
passivation. The passivation is one of the most common methods used in stainless steels (SS), increasing
the resistance of steel against corrosion [1-4].
The classification of stainless steels can be divided according to the microstructure, austenitic
(γ), ferritic (α), duplex (α+γ), precipitation hardening (PH), and martensitic (γ’) [1, 5-6]. Due to the good
performance in critical conditions, the aeronautical industry employs PH, martensitic, and austenitic in
actuators, landing gear supports, and fasteners [6, 8].
The PH stainless steels (PHSS) have excellent corrosion resistance, and heat treatment can be
applied to change mechanical and corrosion properties. The PHSS are divided into semi-austenitic,
austenitic, and martensitic [9-16].
Several types of research on SS are focused on calculated corrosion rates, pitting potentials,
corrosion mechanisms, and passive-transpassive regions of passivation samples employing
potentiodynamic polarization (PP), electrochemical impedance spectroscopy (EIS), galvanodynamic
polarization (GP), and electrochemical noise (EN) techniques [17-20].
The advantages of working with the electrochemical noise technique are that it is a non-
perturbative test and describes the electrochemical processes that occur when current or potential change
can be fluctuations or transients [21-23]. The transients can explain different reactions, such as cathodic
or anodic, related to the passive film's rupture and regeneration. Also, continuous transients can be
related to pitting formation and propagation [25-26]. Another EN advantage is that it provides valuable
information about the process of localized corrosion.
Factors such as the working electrodes' surface area, electrode symmetry, and electrolyte
resistance directly influence EN measurement. Diverses authors suggested different methods to study
EN data. The methods are divided into frequency domain, time-domain, and time-frequency domain.
The time-domain methods are more common to study and consist of analyses of statistical parameters
such as skewness, Kurtosis, noise resistance, localization index (LI), and standard deviation; those
analyses are the most reported. The frequency-domain analysis consists of transform signals as FFT (fast
Fourier transforms) for PSD (power spectral density), shot noise, and noise impedance. Finally, time-
frequency-domains study the HHT (Hilbert-Huang transform), Stockwell transform, DWT (discrete
wavelet transform), Shannon entropy, etc [27-30].
Suresh and Mudali [31] investigated the AISI 304 SS by applying EN determinating localized
corrosion when AISI 304 is in FeCl3. Lara et al. [32] characterized PHSS (15-5 and 17-4) by EN and
PPC techniques obtaining that the oxide layer generated in both media is similar. Bragaglia et al. [33]
employed PP in 304 AISI SS with passivation and uncoated. The results showed an increase in pitting
potential for passivated samples related to using nitric acid as a passivation electrolyte. Marcelin et al.
[34] studied that a passive layer was formed by air exposition. And other authors characterized the
electrochemical behavior of PHSS by employing EIS and EN [35]. The results showed that CUSTOM
450 PHSS has better properties against corrosion. Elements such as chromium increase the corrosion
 Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 3

resistance in PHSS by generating a Cr2O3 layer [36-37]. One way to obtain this oxide layer is by
passivation, based on ASTM A967 [22].
This work aims to characterize the AM350 PHSS in nitric and citric acid passivation electrolytes
at 49 and 70°C at different exposure times (50 min) in 5 wt. % NaCl and 1 wt. % H 2SO4 solutions uses
electrochemical noise (EN) technique.

2. MATERIALS AND METHODS

2.1. Materials

The material used in this work was AM350 (UNS35000) stainless steel. The nominal chemical
composition of this stainless steel [35] is shown in Table 1.

Table 1. Chemical composition of the AM350 SS (wt. %).

Alloy Fe Cr Ni Mo Mn Cu Ti Nb N Si C S
AM350 Balance 16.0– 4.0– 2.50– 0.50– – – – 0.07- ≤0.50 0.07– 0.030
17.0 5.0 3.25 1.25 0.13 0.11

2.2 Passivation Treatment

The passivation was made it followed the ASTM A9677-17 and ASTM A380-17 specifications
regulating the pretreatment [degreased and pickling in a 50 wt.% HCl for 5 s at 25 °C and rinsed in
distilled water], Passivation treatment [passivation baths, passivation time and temperature], and final
treatment [Rinsed in distilled water] [22, 37]. A DoE 5 (design of experiments) was employed due to the
acid combinations, concentration, temperature, and passivation time, See Figure 1. Table 2 shows the
parameters of passivation treatment for each type of PHSS.

Table 2. Nomenclature and passivation treatment parameters.

Nomenclature Passivation Time Temperature

PHSS
samples * Baths (min) (°C)
CA-50min-49 °C Citric acid - C6H8O7 49
NA-50min-70 °C Nitric acid - HNO3 70
AM 350 50
NA-50min-70 °C Nitric acid - HNO3 70
CA-50min-49 °C Citric acid - C6H8O7 49
* Citric acid (CA) and Nitric acid (NA)
Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 4

Figure 1. Diagram of passivation treatment of AM 350 PHSS. Two passivation baths of nitric acid
(20%v) and citric acid (55%v) solutions were used. A constant temperature of 49 and 70 °C was
maintained through the passivation treatment. Specimens were immersed in the solutions for 50
min.

2.3. Microstructural Characterization

AM 350 samples were prepared by metallography technique. The grinding was made with SiC
sandpaper (from 400 to 800 grade) to be cleaned for 10 minutes in ultrasonic with ethanol and deionized
water [38].
The microstructure was determined by optical microscopy (OM) and scanning electron
microscopy (SEM, JEOL-JSM-5610) with secondary electrons (SE) at 500× and 2000×.

2.4. Electrochemical Test

2.4.1. Electrochemical Noise

The EN characterization was made of 1024 data, 1 data per second. The cell array consisted of
three electrodes, the working electrode (AM350), the reference electrode (SCE), and a platinum wire of
the working electrode 2. The data were filtered with the polynomial method (9°). Power Spectral
Density, polynomial filter, and wavelet transformed were applied using a MATLAB 2018a program. All
measurements were based on ASTM G199-09 and triplicate [39-41].

2.4.1.1. Polynomial Method

The trend signal (DC) separation is necessary to eliminate interference signals for the different
EN analysis methods. To obtain a filtered signal (yn) is necessary to apply a polynomial (po) of grade
“n” at n-th term (ai) [42].

𝑝
𝑜
𝑦𝑛 = 𝑥𝑛 − ∑𝑖=0 𝑎𝑖 𝑛𝑖 (1)
Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 5

2.4.1.2. Power Spectral Density (PSD)

The PSD signal is calculated using the FFT (fast Fourier transform) to a filtered signal, in this
case, the current signal.

1
R xx (m) = N ∑N−m−1
n=0 x(n) · x(n + m), for m positve values (2)
−2πkn2
γ·tm
Ψx (k) = · ∑N
n=1(xn − x
̅n) · e N (3)
N

To interpret PSD is necessary to study the slope specter value, which helps to relate the corrosion
type of the system. The following equation calculates the slope (βx):
𝑙𝑜𝑔𝛹𝑥 = −𝛽𝑥 𝑙𝑜𝑔 𝑓 (4)
Also, ψ0 (frequency zero limits) can give information about material dissolution when it is
analyzed in the current. Table 3 gives the slope values related to different corrosion types [43].

Table 3. Intervals of β to determine the corrosion type [43].

Corrosion type
Units Scale
Uniform Pitting Passive
Minimum 0 7 1
dB(A)·decade-1
Maximum 7 14 1

2.4.1.3. Wavelets Method

The wavelets method helps decompose a signal according to the frequency of the process,
dividing it into long, middle, and fast processes. The energy (fraction) is divided into crystals. The first
and middle crystals are related to the localized process (D1-D6), and the final crystals are related to the
controlled, diffusion, or generalized process due to a long-time duration [44-47].

𝐸 = ∑𝑁 2
𝑛−1 𝑥𝑛 (5)

1 1
𝐸𝐷𝑗𝑑 = 𝐸 ∑𝑁 2 𝑠 𝑁 2
𝑛=1 𝑑𝑗,𝑛 𝐸𝐷𝑗 = 𝐸 ∑𝑛=1 𝑠𝑗,𝑛 (6)

𝑗
𝐸 = 𝐸𝐷𝑗𝑠 ∑𝑗=1 𝐸𝐷𝑗𝑑 (7)

Table 4 shows the crystals' range scale in seconds and Hz [44].

Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 6

Table 4. Ranges of crystals scale

Scale Scale
Crystal (D)
(s) (Hz)
1 1-2 1 - 0.5
2 2-4 0.5 - 0.25
3 4-8 0.25 - 0.125
4 8 -16 0.125 - 0.0625
5 16 - 32 0.0625 - 0.3125
6 32 - 64 0.03125 - 0.015625
7 64 - 128 0.015625 - 0.00781
8 128 - 256 0.00781 - 0.00390

3. RESULTS AND DISCUSSION

3.1. OM-SEM microstructural

Figure 2 shows the microstructures obtained by OM and SEM-SE analysis. Figure 2a shows the
microstructure by OM; the austenitic phase is present in microstructure of AM350 with the delta (δ)
ferrite phase. In figure 2b, the microstructure by SEM corroborates the results. [49-50].

Figure 2. Microstructure of AM 350 precipitation hardening stainless steel (initial conditions): (a)
Optical microscopy (OM) and (b) scanning electron microscopy with secondary electrons SEM-
SE

The pitting resistance equivalent number (PREN) is related with pitting corrosion and helps to
compare different SS pitting tendencies [51-53]. If PREN is high is related to high resistance against
pitting corrosion. PREN can be determined with the following equation:

PREN = Cr + 3.3Mo + 16N (8)

Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 7

Table 5. Pitting resistance equivalent number (PREN) analysis of AM350.

PHSS Cr Mo N PREN
AM350 16.0–17.0 2.50–3.25 0.07-0.13 25.37

3.1. Electrochemical measurements

3.1.1. Electrochemical Noise

Figure 3a and 4a shows the time series of passivate steels exposed to NaCl electrolyte. The
electrochemical potential noise (EPN) is presented in figure 3a. All the samples showed a decrease in
voltage amplitude in time function. The reduction of amplitude is related to the stabilization of ionic
exchange. The sample NA-50min-70 C presented amplitudes of 3×102 V, the higher demand. Also, the
electrochemical current noise (ECN) from figure 4a showed that sample NA-50min-70°C has a higher
current amplitude (3×106 A·cm2). This behavior is related to increase in corrosion kinetic. The sample
CA-50min-49°C showed a similar behavior but amplitudes of 1×106 A·cm2, meaning that resistance
to charge transference is higher. However, as time passes, the sample passivated in nitric acid reduces
the current demand, reducing ion and charge transference due to a more stable passive layer. The relation
between the current and potential is necessary to obtain corrosion resistance [54-55].

Figure 3. Electrochemical potential noise (EPN), for AM350 passivated stainless steels immersed in (a)
5 wt. % NaCl and (b) 1 wt. % H2SO4 solutions.

The EPN series of figure 3b shows the behavior of passivate steels exposed in H2SO4. Both
samples presented low amplitudes (2×104 V). The low fluctuation can be related to the generation of
the passive layer. In ECN of figure 4b, the samples presented transients. However, the transients were
Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 8

of low amplitude for NA-50min-70°C (3×107 A·cm2), while for CA-50min-49°C, the transients were
of 1.4×106 A·cm2. This behavior can be related to localized corrosion due to breaking and regenerating
the passive layer or breaking and pitting of material.

Figure 4. Electrochemical current noise (ECN)–time series, for AM 350 passivated stainless steels
immersed in (a) 5 wt. % NaCl and (b) 1 wt. % H2SO4 solutions.

3.1.1.1. Statistical Analysis

The statistical analysis shows that samples in NaCl presented uniform corrosion. When
passivated samples were exposed to H2SO4 presented localized and mixed corrosion. The results
obtained by skewness corroborated the LI results in both electrolytes (see table 6). It is essential to
mention that samples anodized in nitric acid presented a higher noise resistance, meaning a higher
resistance against corrosion. [56-57]

Table 6. Electrochemical noise statistical parameters from passivated AM 350 stainless steels immersed
in 5 wt. % NaCl and 1 wt. % H2SO4 solutions.

Noise
Location
Resistance Type of Type of
Solutions Samples Index Skewness
Rn Corrosion Corrosion
LI
(ohm)
Sodium NA-50min-70 °C 873.0 0.009 Uni −0.23 Uni
Chloride
(NaCl) CA-50min-49 °C 3047.0 0.003 Uni 0.14 Uni
Sulfuric NA-50min-70 °C 1571.0 0.20 Loc 1.70 Loc
Acid
(H2SO4) CA-50min-49 °C 1055.0 0.04 Mix 2.40 Loc
Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 9

3.1.1.2 Power Spectral Density Analysis and Noise Impedance (Zn)

Figure 5a shows the PSD of the ECN signal. Both samples present a similar Ψ0 value (129 dBi).
Also, the behavior of slope in all frequencies is very similar, 12 and 14, related to a pitting corrosion
process. In figure 6a, the value of Zn0 of NA-50min-70°C is 75386 Ω·cm2, and of CA-50min-49°C is
25491 Ω·cm2, meaning a higher corrosion resistance for sample anodized in nitric acid. [55, 58-59]

Figure 5. Power spectral density (PSD) for AM 350 passivated stainless steels immersed in (a) 5 wt. %
NaCl and (b) 1 wt. % H2SO4 solutions.

Figure 5b shows de PSD of ECN in H2SO4. In this case sample anodized in citric acid presented
a higher value of Ψ0 and In figure 6b the lower Zn0 (128 dBi and 3832 Ω·cm2), meaning that corrosion
kinetic is higher than anodized with nitric acid. However, both samples presented slope values related
to uniform corrosion. However, some changes in slope at high frequencies can be related to an unstable
passive layer. The results obtained by this method is related to a passive layer development and the
regeneration of this one.
The results obtained by Zn0 correspond to the noise resistance (Rn) from tables 6 and 7,
respectively, indicating a close relation between noise impedance and noise resistance from the
frequency and time domain. Diverse authors [60-62] associated the two resistances with homologous
with Rp, but with the EN technique.
Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 10

Figure 6. Noise impedance (Zn) for AM 350 passivated stainless steels immersed in 5 wt. % NaCl and
1 wt. % H2SO4 solutions.

Table 7 shows the PSD parameters. Pitting corrosion in NaCl electrolyte can be related to the Cl
ions that attack the passivated surface. However, the values obtained by slope values differed from those
obtained by statistical analysis. For this reason, another analysis method must be employed to
corroborate the type of corrosion occurring on the surface. Almeraya et al. [55] mentioned that this class
of passivate presented higher corrosion rates when were exposed in sulfuric acid. This behavior can be
related with the OH reaction on passivate surface, dissolving easier the passivate and also part of PHSS.

Table 7. Parameters obtained by Power Spectral Density Analysis and Noise Impedance (Zn).

Noise Frequency
Slope
impedance Type of Zero
Solutions Samples Β
Zn0 Corrosion Ψ0
(dB (A))
(Ω·cm2) (dBi)
Sodium AM350-NA-50min-70°C −14 75386 Loc −129.557
Chloride
(NaCl) AM350-CA-50min-49°C −12 25491 Loc −129.978

Sulfuric Acid AM350-NA-50min-70°C 2 12574 Uni −147.885

(H2SO4) AM350-CA-50min-49°C 1 3832 Uni −128.661

3.1.1.3. Wavelets Analysis

Figure 7 shows the EDP (energy dispersion plot) of AM350 passivate in passivation samples.
When samples were exposed to NaCl (figure 7a), both samples presented a higher energy accumulation
in crystals D7 and D8. Those crystals are associated with a process of long duration as uniform corrosion
of diffusion (species or pitting). On the other hand, when samples are exposed to H2SO4 (figure 7b), the
Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 11

steel passivated in nitric acid presented high accumulation of in crystals the first three and D8. This
behavior is associated to a possible pitting diffusion due to an unstable passive layer. The steel passivated
in citric acid presented a higher energy accumulation in the last crystals (D7 and D8), related the process
with uniform corrosion [3, 63-64].

Figure 7. Energy Dispersion Plot (EDP) calculated by wavelets method for AM 350 passivated stainless
steels immersed in (a) 5 wt. % NaCl and (b) 1 wt. % H2SO4 solutions.

3.2. SEM microstructural analysis

Figure 8 shows the SEM analysis of samples after the EN test. Figure 8 a-b shows the damage
caused by NaCl. Both samples presented the pitting process, but the pitting was distributed uniformly,
related to a pitting diffusion on the surface. Also, pitting is in micrometers' order.
The results matched with the EDP from figure 7a, where a long-time process (diffusion) is
present in both samples. Figure 8 c-d show the damage caused by H2SO4. Figure 8c shows one significant
pitting surrounded by minor pitting. This behavior can be associated with pitting nucleation in figure 6b,
where NA-50min-70°C presented high energy in the first crystals. However, the minor pitting around
the biggest meaning is the begging of a diffusion process. For that reason, figure 7b showed a high
energy accumulation in D7 and D8 crystals for NA-50min-70°C, so pitting diffusion is slower for this
sample. The behavior presented for passivated in citric acid is of pitting diffusion around the biggest
pitting. [3, 44, 65]
Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 12

Figure 8. SEM-SE analysis of AM 350 PHSS immersed in 5 wt. % NaCl solution (a) NA-50min-70°C
and (b) CA-50min-49°C. In 1 wt. % H2SO4 solution (c) NA-50min-70°C and (d) CA-50min-
49°C.

4. CONCLUSIONS

o The results indicated that the passivated in citric acid does not generate a better passive
layer than in nitric acid. This behavior is related to a high presence of chromium oxide in
the passive layer because nitric acid can generate chromium oxide more easily than citric
acid. However, those results do not mean that citric acid is a bad option to passivate
samples, but in AM350, PHSS is not better than nitric acid passivation.
o For the passivate samples, statistical and wavelets analysis presented a better option to
determine the surface corrosion type.
o Also, statistical analysis can be a good option to study passivate SS in electrochemical
noise.
o The results in the time-frequency domain indicate that the alloy passivate in nitric acid
exposed in H2SO4 presented high energy accumulation in the first crystals; this behavior
can be related to a localized process propitious by nitric acid passivation.
o The values of noise resistance (Rn) and noise impedance (Zn0) can be cataloged as
homologous due to their similar behavior, reflecting the relation with corrosion rate.
o The aggressive H2SO4 is related to the lower corrosion resistance values. Also, it means
that the passive layer can be diluted in the electrolyte; also, the anodized in citric acid can
Int. J. Electrochem. Sci., 17 (2022) Article Number: 220950 13

be diluted easier than in nitric acid.

o SEM postmortem analysis corroborates the results of the wavelets and statistical methods.
Also, the SEM figure shows a predominance of pitting diffusion and nucleation on the
surface of passivating samples.

ACKNOWLEDGMENTS
The authors thank the Mexican National Council for Science and Technology (CONACYT) for
supporting the projects A1-S-8882, the UANL-CA-316 working group, and Universidad Autónoma de
Nuevo León (UANL) for the facilities given to developing this investigation and the technical assistance
from M. Sc. Luis G. Silva Vidaurri.

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