Enhanced Electrochemical and Corrosion Behavior of Amorphous 316-type Stainless Steel Microfibers in Saline Environment

doi:10.21203/rs.3.rs-2443500/v1

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Enhanced Electrochemical and Corrosion Behavior of Amorphous 316-type Stainless Steel Microfibers in Saline Environment

https://doi.org/10.21203/rs.3.rs-2443500/v1

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The resistance of commercial stainless steel (SS) types in harsh environments is problematic because of the breakdown of the passive chromium oxide layer. This study reports fully amorphized 316 SS microfibers using a customized multi-nozzled melt-spinning technique. Electrochemical tests in 3.5 wt.% NaCl shows a high corrosion resistance with an annual corrosion rate of less than 60 µm year^–1 under ambient conditions, which increases slightly as the temperature rises to 50°C. The room temperature sample also shows a low passivation current at the level of 10^–4 A cm^–2 with long-term stability, and no pitting is observed for all the samples until 1.5 V. The sample polarized at 37°C shows the smallest bulk resistance (~ 1400 Ω cm²) and the largest double-layer capacitance (28.6 µF cm^–2), where large amounts of salt accumulation on the surface creating a passive layer on the microfibers were detected by energy dispersive X-ray (EDX)–scanning electron microscopy. Cross-sectional investigation by EDX-scanning transmission electron microscopy corroborates the homogenous bulk composition and Fe-rich, Ni and Cr-containing amorphous oxides, both of which contribute to the enhanced corrosion and passivation properties compared to commercial SS counterparts in the literature.

Physical sciences/Materials science/Materials for energy and catalysis/Electrochemistry/Corrosion

Physical sciences/Materials science/Condensed matter physics/Surfaces interfaces and thin films

The corrosion behavior of state-of-the-art conventional metals and alloys in simulated saline environments has garnered particular interest where automotive/marine parts, offshore infrastructure, prosthetics/implants, and coatings suffer from degradation of their mechanical properties over time^1–7. A commonly used material, stainless steel, is known to have high strength and durability, containing a passive chromium oxide film on the surface; however, it corrodes over time in a saline environment due to the breakdown of the passivity^8,9. For better corrosion protection in a saline environment, magnetron-sputtered NiNb thin film coatings were utilized on 316 SS to form a stable Nb₂O₅ passive film¹⁰. In another study, ZrN thin film coating by unbalanced magnetron sputtering on 304 SS increased the passivation behavior by at least 100 times relative to bare 304 SS by looking at the decrease in the corrosion current density¹¹. Besides, titanizing¹², gamma-alumina¹³, zirconia^14,15, titanium boron nitride thin films¹⁶, WO₃ nanoflakes coated with TiO₂ nanoparticles¹⁷, borate glass¹⁸, amorphous boron¹⁹, amorphous hybrid silane reinforced with ZnO²⁰, FeCo₂O₄ nanowire arrays²¹, polypyrrole-sulfonated melamine formaldehyde nanocomposites²², polypyrrole doped with dodecylbenzenesulphonic acid²³, polypyrrole-Al₂O₃ composite²⁴, poly(vinylcarbazole)/alumina nanocomposite²⁵, polyterthiophene²⁶, polyaniline and its derivatives²⁷, superhydrophobic electroactive epoxy²⁸, polyaniline-graphene oxide²⁹, nickel hydroxide-graphene oxide³⁰, carbon nanotube/nanofiber³¹, organic-inorganic hybrid sol-gel silica³² are coated on 316 series stainless steels to improve their performance for a range of applications. Temperature increase directly results in a higher corrosion rate of steels, accounting for faster electrochemical reactions due to additional energy input at relatively higher temperatures³³.

Despite the fact that 316 stainless steels (SS) are widely used in construction and marine industries, the remarkable electrochemical activity in the media containing aggressive environments containing chloride and fluorine ions makes them susceptible to corrosion^10,34,35. There are also studies evaluating the chloride corrosion behavior of 316-type SS in heating pipelines³⁶ and heat-exchanging surfaces³⁷. In fact, the amount of Cl^– ions adsorbed on the surface determines the localized corrosion and anodic dissolution processes³⁸. It was previously suggested that Cl^– ions react with the oxide layer, penetrate into the passive film, and occupy oxygen vacancy sites³⁹. Cl^– ions can then migrate and react with the metal-oxide interface⁴⁰. The formed metal chloride (probably Cr is the main element interacting with Cl)⁴¹ expands and breaks the oxide film, rendering a rapid penetration of Cl^– and in turn, localized corrosion⁴². It is also known that the formation of hydrated iron oxide and pitting corrosion of chlorides, sulfates, fluorides, nitrates, and so forth expands steel bars, generating internal pressure in the surrounding concrete, which in turn causes structural degradation in the carcass of the buildings⁴³. To overcome this drawback, microfilament steel (MS) fibers with low fiber content are incorporated into concrete⁴⁴. Compared to mono-fiber reinforced concretes (FRC) with a steel bar, MS-containing FRCs have superior strength and a better dispersion index compared to synthetic polymer-reinforced FRCs due to minimum entanglement observed between the embedded steel microfibers.

Among iron systems, amorphous Fe-based alloys are counted to be one of the best-performing materials because of their superior corrosion and wear resistance and relatively low cost compared to their crystalline counterparts^45–53. The biocorrosion of amorphous Fe-based alloys was studied in different biological solutions, including artificial saliva and phosphate-buffered saline, where the passive behavior in these media makes them ideal candidates for orthopedic and dental applications⁵⁴. There is a considerable number of reports in the literature on the synthesis and characterization of amorphous micro/nanofibers^55–59. Our recent study demonstrated a new method of ejecting individual melt droplets on a rotating wheel to produce commercial 316 SS (DIN 1.4401) amorphous stainless steel thin films that are fragmented into amorphous microfibers upon solidification⁶⁰. The produced amorphous ribbons were shown to have more than twice the hardness of their polycrystalline stainless-steel counterpart. The present study evaluates the corrosion properties and passivation kinetics of 316 amorphous stainless steel in an aqueous 3.5% NaCl solution. The morphological properties before and after linear sweep voltammetry (LSV) are analyzed through ultra-high resolution scanning electron microscopy imaging. The electrochemical studies suggest that the resistance to corrosion in the presence of chloride is significantly improved by forming fully amorphous stainless steel microfibers without the need for an external coating.

Fabrication of amorphous 316 stainless steel microfibers

Figure 1a depicts schematics of the nanofiber formation process by the customized melt-spinning device with a multi-slit nozzle with an opening of ~ 30 µm. After the metal ingot becomes molten, with the aid of pressure, the material is ejected out of the nozzles (stage I). Due to high surface tension, melt droplets form at the exit of the slit nozzle openings, which later on wet the rotating copper wheel and form a thin film structure (stage II). As the thin film leaves the copper wheel, it fragments into microfibers due to void nucleation and growth within the film (stage III) ⁶⁰. The real-life melting and microfiber production is shown in Fig. 1b. A stack of produced microfibers and an SEM image of a representative fiber are displayed in Fig. 1c,d, respectively. The characteristic maze-like pattern obtained from the TEM image (Fig. 1e), the corresponding selected area electron diffraction (SAED) of the bulk sample with broad halo (Fig. 1e – inset), and the overall X-ray diffractogram in Fig. 1f confirm its fully amorphous state. The amorphous state stems from the quenching rate of the modified melt spinning technique was theoretically calculated to be two orders of magnitude higher (up to 10⁸ K s^–1) than the quenching rate of conventional melt spinning ^60–62.

Electrochemical behavior

The behavior of the as-quenched DIN 1.4401 (Type 316) amorphous stainless steel microfibers at three different temperatures (25, 37 and 50°C) is depicted in Fig. 2a. The corrosion potential, E_corr, shifts from ~ 0.075 V to −0.240 V as the temperature increases, which is because the reactivity of the material is increased in a saline environment. For the 25°C sample, passivation starts at relatively lower current densities, j_pass, compared to the 37°C sample. For the 25°C samples, the double layer induces a potential barrier to the passage of ions which causes a remarkable improvement in passivation kinetics^63,64. We do not observe a clear passivation region for the 50°C sample, as confirmed by the rise in the current density in the anodic part with many current jumps. This could be linked to enhanced metal-chloride ion interactions at this temperature. Pitting is not observed in any of the samples until 1.5 V, indicating their extended passive region compared to other stainless steel bulk materials and coatings with the same or different compositions in the literature^65–69. In the cathodic part, after the hump observed at −0.75 V, the steepness of the decrease in the current density increases, and the curve attains a more symmetric shape in the near-equilibrium region close to the open circuit potential. As expected, the ACR shows a slight increase with increasing solution temperature (Table 1). To confirm the stability of the material in this region, chronoamperometric analysis at a constant potential of 0.15 V for 3 h at 37°C was conducted (Fig. 2b). The results show that although there are sudden changes in the current density at the beginning of the experiment, the system reaches a plateau after ~ 1h, thus confirming that the considered stainless steel microfibers reach stability in the simulated seawater.

Table 1

Corrosion properties of DIN 1.4401 amorphous stainless steel microfibers at 25, 37 and 50°C. J_corr: corrosion current density, E_corr: corrosion potential, J_pass: passivation current density, *ACR*: annual corrosion rate. Note that the maximum standard deviation values are presented.
Temperature (°C)	J_corr (A cm^–2) ±0.03 ⋅10⁻⁵	E_corr (V vs Ag/AgCl) ±0.001	ACR (µm yr^–1) ±2.3	J_pass (A cm^–2) ±0.05 ⋅10⁻⁴
25	7.74⋅10⁻⁶	0.075	59.3	5.48 ⋅ 10⁻⁴
37	9.24⋅10⁻⁶	−0.048	70.8	2.64 ⋅ 10⁻³
50	1.00⋅10⁻⁵	−0.240	76.6	N/A

The Nyquist plots present the behavior of the material before and after polarization at different temperatures (Fig. 3a). The bulk resistance, R_b, can be estimated from the Nyquist plot (either a perfect or a depressed semicircle) using the following Eq. 2 ⁷⁰:

$\left|Z\right|=\sqrt{{\left({Z}_{\text{r}\text{e}}\right)}^{2}+{{(Z}_{\text{i}\text{m}})}^{2}}=\frac{{R}_{\text{b}}}{2}$ at ${f}^{{Z}_{im\_max}}$. (2)

Hence, the ${R}_{\text{b}}$ values for each measurement are estimated and given in Table 2. ${R}_{\text{b}}$ rises exponentially with the increase in the test temperature from 25°C to 50°C linked to the existence of Na⁺ and Cl^– ions at the surface, which do not permit fast electron transfer. However, the surface becomes significantly more active with the coating of the salt ions on the surface upon polarization, where the most active surface is observed at 37°C with the smallest ${R}_{\text{b}}$.

The theoretical limit of the highest impedance is determined from the characteristic angular frequency ${\omega }_{0}$ in Eq. (3):

$${\omega }_{0}=2\pi {f}_{0}=1/\left({R}_{\text{b}}*{C}_{\text{d}\text{l}}\right)$$

where ${f}_{0}$ is the characteristic frequency obtained from Fig. 3b. Hence the double-layer capacitance, ${C}_{\text{d}\text{l}}$, can be obtained (Table 2). The sample at 37°C has the largest ${C}_{\text{d}\text{l}}$ accounting for the considerable accumulation of ions on the material surface at this temperature.

Microstructural and compositional analyses

For both 25 and 37°C samples, ${C}_{\text{d}\text{l}}$ drops significantly after polarization, which could be because of the electron transfer of the Na⁺ and Cl^– ions to the material and hence the formation of large amounts and sizes of NaCl particles (either irregular-shaped small particles or large particles with solid corners) on the surface (see Fig. 4a,b for the 25°C and Fig. 4c,d for the 37°C samples). On the other hand, the 50°C sample shows an increase in ${C}_{\text{d}\text{l}}$ after polarization. SEM images of the as-polarized sample show only accumulated granule-type NaCl particles (Fig. 4e). Small cracks and porosity indicate that the salt reacts with the material at this temperature (Fig. 4e,f), which also explains the unstable passivation plateau displayed in Fig. 2a.

Table 2

Bulk resistance R_b and double-layer capacitance C_dl of the electrodes in 3.5% NaCl solution before and after polarization.
	25°C_before	25°C_after	37°C_before	37°C_after	50°C_before	50°C_after
R_b (Ω cm²)	52470 ± 1456	6462 ± 183	66554 ± 1464	1412 ± 29	251228 ± 4068	6528 ± 205
C_dl (µF cm²)	9.58 ± 0.26	1.55 ± 0.04	189.94 ± 0.54	28.59 ± 0.58	0.79 ± 0.01	4.90 ± 0.15

An example of the composition analysis performed after polarization at 37°C depicts the containing elements (Fig. 5b-g) and a remarkable local NaCl accumulation on the surface (Fig. 5f-g). Although oxygen can be observed all across the sample and the outer regions (Fig. 5a), no visible oxygen is observed on the NaCl particles, indicating that oxide formation during polarization does not play a role in the changes in the electrochemical behavior (Fig. 5a). After cleaning, NaCl is gone, and the sample has an even surface composition (Fig. 5b). Hence, it can be deduced that the sample is not influenced by the electrochemical polarization test.

Figure 6a shows a cross-sectional HAADF-STEM image of the amorphous 316 SS microfibers (C, S, and P are excluded because of the negligible quantities within the material). A region with a thickness of ~ 2 nm with a relatively darker contrast on the bulk sample can be clearly observed from the HAADF image. EDX mapping reveals that this region is rich in oxygen. Line scan across the sample (Fig. 6b) corroborates that this oxide mainly contains Fe (55 at.%), Cr (13 at.%) and Ni (8 at.%), and the FFT pattern (Fig. 6b inset) with broad halos corroborates the amorphous state of the oxide film and bulk phase.

This study reveals the high corrosion resistance and electrochemical stability of commercial 316-type stainless steel produced in the form of amorphous microfibers by melt-spinning of molten steel ingot passing through the multi-slit nozzle. The fully amorphous state realized by the extremely high cooling rates upon melt spinning is confirmed locally by the selected area electron diffraction and globally for a bundle of microfibers by X-ray diffraction. The corrosion current density is ~ 7.7 ⋅ 10⁻⁶ A cm^–2 at 25°C (annual corrosion rate, ACR, of ~ 59.3 µm year⁻¹) and as the temperature increases to 50°C, this value becomes 10⁻⁵ A cm^–2 (~ 76.6 µm year⁻¹). For the 50°C sample, due to enhanced metal-chloride interactions at relatively more positive potentials, a steady increase in terms of potential is observed that does not permit a clear passivation region. The long-term stability of the room temperature samples was confirmed by keeping the material right below the polarization region (0.15 V) for 3 h. Most importantly, for every temperature measured until 1.5 V, a passive region without pitting is observed; hence the corrosion properties of the amorphized 316 SS are better than many other polycrystalline stainless steel bulk materials and coatings in the literature. The surface interactions remarkably increase with the accumulation the salt ions on the surface during polarization, where the most active surface is determined for the sample polarized at 37°C exhibiting the smallest bulk resistance and largest double layer capacitance. A remarkable local NaCl accumulation on the surface is observed at that temperature, as confirmed by scanning electron microscopy imaging. On the other hand, no detectable oxygen content was observed on the NaCl particles in any of the examined samples via energy-dispersive X-ray mapping, indicating that the influence of oxide formation is negligible for the changes of R_b and C_dl. Scanning transmission electron microscopy investigation on an as-spun sample confirms a less than 2 µm thick Fe-rich, Cr and Ni-containing oxygen on the surface, which could be why the material is resistant to pitting corrosion for extended anodic polarization. Hence, the findings of these studies suggest that microfibers of amorphous stainless steel can be used in different engineering applications, e.g., in reinforced composite forms, with improved anti-corrosive behavior.

Melt spinning of microfibers. The production of microfibers was achieved using a custom-built melt-spinning device, which includes a boron nitride crucible (diameter: 18 mm, length: 95 mm, INNOVACERA, China) with a slit nozzle opening of 0.03 mm². Crystalline bulk 316-type (DIN 1.4401) was purchased from Advent Research Materials, England. The chamber was evacuated to 10^–6 mbar and subsequently purged three times with argon (800 mbar with > 99.999% purity). The linear speed of the copper wheel and its distance to the nozzle opening was selected as 63 m s^–1 and 150 µm, respectively. The 316-type bulk ingot was heated to 1550°C, above its liquidus temperature, and ejected through the nozzle in droplet form into the 800 mbar argon-filled chamber by applying an argon overpressure of 1200 mbar.

Electrochemical tests. A 3.5 wt.% aqueous Ar-aerated NaCl solution with a pH = 5.2 was used in this study. The electrochemical measurements were conducted in a three-electrode glass cell at 37°C using a Pt counter electrode (0.5 mm diameter) and Ag(s) /AgCl(s) reference electrode with 3 M NaCl electrolyte and an ion-permeable porous glass junction that has a redox potential of + 0.195 V (at room temperature) vs. a reference hydrogen electrode. A bundle of 14–15 electrodes was wrapped firmly from one side by a conductive silver paint and copper foil, and part of the microfibers was immersed into the electrolyte. The electrochemical measurements were performed with a Gamry Interface 1010e Potentiostat/Galvanostat/ZRA. Before the electrochemical tests, an open circuit potential (OCP) was applied for 3600 s to confirm the stabilization of the working electrode/electrolyte interface. Chronoamperometric measurements were carried out at 0.15 V for 3h at 25°C. Electrochemical impedance spectroscopy (EIS) studies were conducted at OCP at an AC amplitude of 10 mV rms recorded from 100000 Hz to 0.1 Hz before the polarization study. LSV was implemented at a scan rate of 5 mV s⁻¹. The forward scan was from −3 V to. +1.5 V vs. Ag/AgCl. The area of the electrodes was estimated from the size distribution given in ref.⁶⁰, with t (thickness) = 5.4 ± 2.3 µm, w (width) = 20.5 ± 17.4 µm (average of round to flat shaped microfibers) and h (submerged height) = 81 ± 8 mm. The areal averaging of the completely flat and round fibers yields 4.089 ± 0.455 mm². DIN 1.4401 stainless steel has a composition: C: 0.07 (max), Mn: 2.00 (max), P: 0.045 (max), S: 0.015 (max), Si: 1 (max), Cr: 16.5 (min) – 18.5 (max) ⁷¹. The theoretical density, ρ ≈ 7.98 g cm^{−3 71}, and the equivalent weight, EW ≈ 18.70, of the considered alloys are calculated using the formulas in ref.⁷². The average annual corrosion rate (ACR) of the samples was calculated using Eq. 1.:

$$ACR=\frac{3.27\times {J}_{\text{c}\text{o}\text{r}\text{r}}\times EW}{\rho }$$

Electron microscopy analysis. The surface and chemical composition of the as-spun, electrochemically-treated, and rinsed microfibers were analyzed by scanning electron microscopy (SEM) using a voltage of 20 kV in a TESCAN VEGA 3 microscope at a working distance of ~ 10 mm and magnifications of 1000⋅ and 2000⋅. Composition mapping was performed with coupled energy dispersive X-ray spectrometry (EDX) at 20 kV, at a spot size of 1.2 µm, working distance and a magnification of ~ 10 mm and 4000⋅, respectively. The information was processed with the software AZtec (OXFORD INSTRUMENTS).

X-ray diffraction. An XPERT-PRO diffractometer with Co K_α X-ray source (λ = 1.7889 Å) was employed. During the experiment, θ − 2 θ scans in Bragg-Brentano geometry with a step size of 0.03° were conducted. To achieve a good signal quality, fiber bundles composed of ~ 50 fibers were used.

Transmission electron microscopy. The cross-section of the specimens was prepared by a focused ion beam (FIB) method using an FEI Helios 600 DualBeam microscope equipped with a field-emission gun electron source and a high-resolution ion column. Prior to FIB, a protective Pt layer was coated on the material surface. In order to eliminate any post-induced crystallization, ion-milling was performed using a GATAN 691 PIPS under low-voltage (0.8 V) conditions. High-resolution transmission electron microscopy (HRTEM), high-angle annular dark field–scanning transmission electron microscopy (HAADF-STEM), and energy-dispersive X-ray spectroscopy (EDX) were captured using a JEM Grand ARM300F microscope with double spherical aberration (Cs) correctors.

Acknowledgements

E.S. thank the innovation program for Marie Skłodowska-Curie Individual Fellowship, with the acronym “MAGIC” and grant agreement No. 892050. J.E. and B.S. are grateful for the support from the Austrian Science Fund (FWF) under project Grant I3937-N36.

Author contributions

B.S. conceived the initial research idea, assisted in the electrochemical tests, and wrote the manuscript. E.S. prepared the microfibers, performed optical microscopy imaging and X-ray diffraction. Y.Z. conducted the HRSTEM analysis. E.Y. performed the scanning electron microscopy and energy dispersive X-ray analyses. A.A. contributed to the electrochemical testing. J. K. and A.S.S. analyzed the data and edited the manuscript. J.E. supervised the project and edited the manuscript.

Competing interests

The authors declare no competing interests.

Data Availability

The datasets used and/or analyzed during the current study are available from the corresponding author on reasonable request.

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Enhanced Electrochemical and Corrosion Behavior of Amorphous 316-type Stainless Steel Microfibers in Saline Environment

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Introduction

Results And Discussion

Fabrication of amorphous 316 stainless steel microfibers

Electrochemical behavior

Microstructural and compositional analyses

Conclusions

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