An Overview on the Corrosion Behavior of Steels Processed by Severe Plastic Deformation

Abstract

Ultrafine grained (UFG) and nanostructured steels have gained attention in the last years because of the possibility of improving both strength and ductility, but also because of their potential for improving several properties in metal applications which allows replacing some conventional steels. The refinement of the microstructure obtained through Severe Plastic Deformation (SPD) has allowed for the improvement of mechanical properties and the performing of several studies related to corrosion control, mitigation, and protection. In this review, the corrosion behavior of ultra-fine grained (UFG) steels is presented regarding the existing literature and the microstructural changes produced through different SPD processes. A focus is placed on the importance of the processes for grain refinement and microstructural changes and, therefore, on the corrosion behavior.

Fig. 1 Low carbon triple-alloyed steel after the HPT process. (a) Ferrite and pearlite are present in the initial condition. (b) Soft ferrite grains probably deformed by dislocation subdivision. (c) Ferrite and Pearlite elongated grains. (d) Development of very small grain size and the deformation of pearlite.⁷⁾

1. Introduction

Reducing the crystalline structure to the nanoscale allows for obtaining high-performance steels for the most demanding applications. For example, carbon UFG steels have been developed for various structural applications including bridges, automobiles, and other strength-critical applications.^1,2) Ultrafine-grained alloyed steels have been designed as advanced high-strength steels for transportation by tailoring complex microstructures including ferrite, austenite, bainite or martensite matrix, or multiphase mixtures.³⁾ Stainless steel has also been studied for improving its properties at room and elevated temperatures for applications in engineering and artistic constructions.⁴⁾ In the case of tool steel, used in harsh environment applications, some studies have also been related to the structure’s refinement to improve its properties.⁵⁾

Several types of steels have been processed using severe plastic deformation (SPD) techniques for obtaining ultrafine grained steels, including carbon steels,^6–11) alloy steels,¹²⁾ stainless steels¹³⁾ and tool steels.¹⁴⁾ The microstructure refinement obtained through these SPD techniques has improved mechanical properties and allowed several studies on corrosion control, mitigation, and protection. Corrosion continues to be a major concern for industries worldwide because of the enormous technical, economic, and social consequences. Highly corrosion-resistant materials are also high-cost materials but can undergo degradation in severe environments or under stress, which explains why it is necessary to use new processing techniques and proper corrosion control strategies.¹⁵⁾

Different types of corrosion can be presented in steels, depending on the chemical mechanism, including uniform or general corrosion, galvanic, pitting,¹⁶⁾ crevice,^17,18) environmentally-induced cracking (stress-corrosion cracking (SCC), corrosion fatigue (CF)),¹⁹⁾ dealloying,²⁰⁾ intergranular and impact-based corrosion (erosion corrosion,^21,22) fretting, cavitation).^23,24) Intergranular corrosion (IGC), also called inter-crystalline corrosion or inter-dendritic corrosion, has been considered the most important mechanism of corrosion in coarse-grained metals, meaning that decreasing grain size in ultra-fine grain steels would decrease the corrosion resistance because of the increase of grain boundaries.

However, many studies have reported ultra-fine and nanocrystalline steels with deteriorated or improved corrosion resistance, which would indicate that different corrosion mechanisms are present and UFG metals and steels, and the corrosion resistance behavior cannot be predicted based on their CG counterparts.¹⁵⁾ In addition, as the steel surface plays such an important role on the corrosion behavior, the processes related to surface severe plastic deformation (S²SPD) need to be taken into account. In this review, the corrosion behavior of ultra-fine grained (UFG) steels is presented regarding the existing literature and the microstructural changes produced through different SPD processes. A focus is placed on the importance of the processes for grain refinement and microstructural changes and, therefore, on the corrosion behavior.

2. Microstructural Changes in Steels Processed by SPD

Severe Plastic Deformation (SPD) modifies the steel microstructure but also causes phase transformations, distribution of impurities and solute elements, segregation, and changes in dislocation density and texture, among others.²⁵⁾ Different techniques of Severe Plastic Deformation have been used to modify the microstructure of the steels and improve corrosion behavior. However, various microstructures can be obtained depending on the initial state of the steel and the processing route.

2.1 Carbon and alloyed steels

Carbon and alloy steels are the most important engineering alloys because they are widely used in many applications. However, they are very susceptible to corrosion environments and require some corrosion control.

Low-carbon and alloyed steels have been processed mainly using Equal Channel Angular Pressing (ECAP) and High-Pressure Torsion (HPT). Low-carbon steels consisting of less than 0.3% carbon^26–28) and low-alloy steels consisting of 0.05–0.25% carbon and other alloying elements, such as Fe–Cr–Ni–Mo,⁶⁾ Fe–Ni–Cr,²⁹⁾ and Fe–Cr,³⁰⁾ have been successfully processed using ECAP. For all the cases the refinement in the microstructure is produced, along with elongated grains with an apparent high dislocation density which affects the mechanical properties with increasing the number of ECAP passes. In these steels, it is expected that soft ferrite experiences larger plastic deformations at the microstructural scale than other phases, i.e., pearlite or cementite, specifically at the boundary between phases. Ferrite is refined by successive subdivisions of dislocation walls due to the operation of multi-slip systems,³¹⁾ mainly at the first stages of ECAP. This same effect has been reported for medium-carbon steels.³²⁾

In interstitial-free (IF) steels, whose carbon content is extremely low, less than 0.003% by weight, the addition of microalloying elements can lead to the formation of carbides and nitrides precipitates. Therefore the ferritic matrix is practically free of carbon and nitrogen interstitial atoms, producing a loss in mechanical strength, which is the main challenge in developing these steels.³³⁾ In IF steels processed by ECAP, significant grain refinement and enhancement in mechanical properties have been reported.^34,35) Higher hardness has been reported when processing these steels using HPT.³⁶⁾ High-manganese austenitic twinning-induced plasticity (TWIP) steels have also been processed using ECAP. A significant increase in mechanical properties was found with elongated grains in the shear direction and many subgrains.³⁷⁾

High-Pressure torsion has also been used to process low and medium-carbon steel, low alloyed, and mild steel.^7,8,38–40) The studies have shown the occurrence of elongated grains and the dissolution of carbide precipitates and other phase colonies such as pearlite and cementite. In Fig. 1, ferrite and pearlite elongated grains for a low-carbon triple alloyed steel are observed, and the complete deformation of pearlite after 5 turns in an HPT process.

Fig. 1

Low carbon triple-alloyed steel after the HPT process. (a) Ferrite and pearlite are present in the initial condition. (b) Soft ferrite grains probably deformed by dislocation subdivision. (c) Ferrite and Pearlite elongated grains. (d) Development of very small grain size and the deformation of pearlite.⁷⁾

TWIP steels processed using HPT have also been studied, and a relationship between the initial grain size and the transformation during deformation has been reported.⁴¹⁾ Accumulative Roll Bonding (ARB) has also been used for processing low and medium-carbon steels because this technique has some advantages, such as a high productivity rate and continuous production.^42,43)

2.2 Stainless steel

Stainless steels (SS) are high alloy steels that contain a minimum of 10.5% chromium, which produces a chromium oxide layer (Cr₂O₃) on the surface that is adherent to the base material and self-healing, explaining why it achieves stainless character. Other alloying elements are added depending on the application, such as nickel, copper, molybdenum, titanium, aluminum, and niobium, among others.⁴⁴⁾ In addition, based on the room temperature microstructure, stainless steel can be martensitic, ferritic, austenitic, and duplex (ferritic-austenitic) and precipitation hardenable stainless steel. Although they have several properties, including good corrosion resistance, they have also been processed using severe plastic deformation to improve their properties.

In martensitic stainless steels, the corrosion resistance is lower than the other types. This steel has been processed using HPT, and the authors found a fully refined structure along with a substantial reduction of dislocations. They also found that the HPT process transformed the full lath martensite into a two phases structure containing martensite and reversed austenite.^45,46) Martensite refinement through ECAP has also shown a significant enhancement in the mechanical properties of martensitic steel.^47,48) Figure 2 shows the refinement of the martensite substructure via ECAP.

Fig. 2

TEM images showing refinement of martensitic substructure via ECAP at different temperatures. Large and refined martensite laths decrease more in size for lower temperatures.⁴⁸⁾

Although ferritic stainless steel has better corrosion resistance than martensitic SS and austenitic SS, SPD processes have improved its mechanical properties and corrosion sensitivity.^49,50) Austenitic stainless steels have austenite (FCC) phase at room temperature, are low stacking fault energy (SFE) materials, and their plastic deformation at low temperatures occurs through several mechanisms simultaneously. These steels have been extensively studied using SPD,^51–56) and it has been shown that various deformation mechanisms are present, depending on the SFE of the material and the processing conditions such as deformation temperature. The initial phase (γ-austenite) gradually transforms to ε- and α′-martensite due to deformation. In this sense, the phase transformations of austenitic steels deformed by SPD by decreasing SFE have been reported as follows: The martensitic transformation (γ → ά_bcc or γ → ε_hcp) is the predominant mechanism when SFE < 20 mJ/m². Twinning occurs when 20 < SFE < 45 mJ/m². For SFE values above 45 mJ/m², plastic deformation is controlled by dislocation slip.^57–60)

Duplex stainless steels consist of a two-phase microstructure of grains of ferritic and austenitic stainless steel (Ferrite + Austenite). In duplex steels processed by ECAP, it has been shown that the appearance of shear bands is favored because the two phases store different magnitudes of deformation, creating a heterogeneous state. In addition, during ECAP, the fraction of austenite declines gradually, and it tends to refine ferrite faster, which is attributed to the twinning deformation mechanism that favors grain fragmentation.^31,61)

2.3 Tool steels

Tool grade steels are generally medium to high alloy steels (0.5%–1.5% carbon content) used for manufacturing parts that require high resistance to wear and/or impact. These steels are used for to manufacture tools intended to modify the shape or dimensions of other materials by cutting, pressing, or grinding. The grain refinement generated by SPD has been little studied on these steels compared to carbon and stainless steels. One of the reasons could be that, being highly alloyed materials, they present high resistance and are difficult to process by SPD (in fact, several SPD dies are manufactured with these steels). Some works have studied the grain refinement, and properties of tool steels processed by SPD.^14,62–64) The tool steel R6M5 was subjected to severe plastic deformation torsion (SPDT), and the influence of the initial state of the tool surface was studied. The refinements of the microstructure were observed along with an increase in microhardness.¹⁴⁾

3. Corrosion Behavior of Steels Processed by SPD

3.1 Carbon and alloyed steels

For these steels, the studies reported agreeing that they behave according to Ralston’s rules for the three modes of corrosion: active, passive, and active/passive. Mild steels and pure steels with ultrafine grains produced by ECAP have been studied using anodic polarization, and the results showed that the two type of steels processed by ECAP present more remarkable passivity because the process contributes to forming of a passive film.^65,66) This passive layer has also been reported for IF gap-free steel processed by ECAP, where a stable passive protective layer in 0.9 mol/L NaOH solution was reported. The pitting potential was used to evaluate the material’s resistance against the formation and growth of corrosion pits, and the results indicate that as the pitting potential increases with ECAP passes, the passive protective layer in the UFG steel is more stable than in the coarse-grain steel.³⁴⁾ This behavior has been found for bulk nanocrystalline pure iron investigated with Electrochemical Impedance Spectroscopy (EIS).⁶⁷⁾ The polarization behavior of IF steels in the active region over a wide pH range controlled by mixing 3.5% NaCl and 0.1 M H₂SO₄ has also been reported, showing that IF nano-grained steels exhibit lower corrosion currents because of the more protective surface layer.⁶⁸⁾ In intersitial free steels, the effect of surface severe plastic deformation (S²PD) has also been studied, and the results show about 55% improvement in the corrosion resistance for the treated samples.⁶⁹⁾

Several studies have also described the corrosion behavior of pure iron and steels with ultra-fine grains.^26,65,70,71) In these cases, the corrosion of UFG metals should be accelerated in active solutions.^71–73) For example, Oguzie et al. reported a bulk nanocrystalline iron produced by severe rolling with lower corrosion resistance than conventional polycrystalline iron ingots in 0.1 and 0.5 mol/L H2SO4 solutions.^72,73) However, several results disagree with this view because other authors showed that the corrosion resistance of a bulk nanocrystalline iron produced by severe rolling was improved in a solution of 1 mol/L HCl or 0.05 mol/L H2SO4 + 0.25 mol/L Na2SO4 compared to the conventional polycrystalline iron ingot.^67,74) It is known that for iron-based alloys, corrosion is generated by forming Fe₃C or Fe₅C₂, which produces a volumetric expansion that produces defects on the surface of the material.^75–77) Guo et al. studied the electrochemical behavior of Fe-iron-based alloys and evidenced the successful improvement of corrosion resistance through near surface-severe plastic deformation (NS-SPD) and thermochemical treatment. After SPD processing, a higher density of dislocations and other defects were generated in the crystal lattice. In addition, the recrystallization process promoted by the thermochemical treatment produced the development of an ultrafine grain structure where dislocations and grain boundaries provided rapid diffusion pathways for Cr that promoted the formation of a protective Cr-rich oxide layer, improving corrosion resistance.⁷⁸⁾

Medium carbon steels, such as 45 and 35 steels subjected to surface mechanical pulse friction treatment (MPT) have shown a more complex behavior, because this treatment, which combines SPD and surface alloying, can both increase or decrease the corrosion rate. The authors showed that steel 45 with a higher content of carbon processed using MPT undergoes corrosion more intensively than the steel 35,⁷⁹⁾ which corresponds to the general rule that an increase in the carbon content of steel increases the corrosion rate.^80,81) However, the MPT process in the 45 steel increases the quantity of retained austenite which can influence the corrosion processes of the metal too. The effect of anticorrosive alloying elements was also studied and the most positive effect on corrosion resistance was for those specimens alloyed with nitrogen, nickel, and boron, showing that the presence of alloying elements not only improves the mechanical properties but also provides anticorrosive properties.^82–84)

3.2 Stainless steel

Stainless steels are the most favored steels for SPD processing. Most of the literature confirms an increase in the corrosion resistance of UFG stainless steels regardless of SPD processing.^{51,57,85–88)} However, not always the corrosion behavior improves in stainless steels, because it also depends on the process and the nanostructured obtained.^30,89) For example, for 316L SS processed using ECAP, a significant improvement in the corrosion behavior has been reported, evidenced by the increase in the polarization resistance and decrease of corrosion rate, the increase in pitting corrosion potential, and the increase of the resistance of the passive film.^90–92) In contrast, Nagaraj et al., studied the tribocorrosion behavior of steel 316L SS processed using ECAP and found a poor corrosion resistance of the treated samples, attributed to the strain accumulation from the ECAP process.⁹³⁾ Rifai et al. investigated the corrosion behavior using the pitting potential of UFG Fe–20% Cr steels processed by ECAP and post-ECAP annealing, and found that the pitting potential of as-ECAP samples was higher at first and decreased with increasing temperature of post-ECAP annealing, because of the increase in grain size.³⁰⁾

The formation and adhesion of passive films on 316L SS processed using HPT have also been reported. The larger amount of grain boundaries, dislocation density, and higher residual stresses provide nucleation sites for the passive oxide layers to become more stable.⁵²⁾ Yusuf et al., combined selective laser melting (SLM) and HPT to process 316 L SS up to 10 turns and obtained a significant porosity reduction in the processed steel, that along with the cellular structure refinement and the homogeneous microstructure contributed to enhancement of corrosion performance.⁹⁴⁾ Zhang et al. also studied the effect of HPT process on 316L steel up to 5 turns without any prior steel treatment, and they found an enhanced corrosion resistance for small deformation (1 turn) because of the increasing in the stability of the passive film, and for large deformation (5 turns) due to dynamic recrystallization and high-density deformation twins. For medium deformation (3 turns), the corrosion resistance deteriorated due to high density dislocations.⁹⁵⁾

Yun-Wei et al. reported the degradation of the corrosion resistance of steel 316 after surface mechanical attrition treatment (SMAT) that produced a nanocrystalline structure. The results showed that the steel surface presented numerous surface cracks that clearly decreased the electrochemical behavior of the material. This result can be seen in the potentiodynamic curves obtained for the steel in the initial state and then processed by SMAT. A higher corrosion current and a lower corrosion potential are evident for the treated steel. However, corrosion resistance improved in this investigation as the annealing temperature increased.⁹⁶⁾ On the other hand, corrosion properties of 316 SS processed using surface mechanical attrition treatment (SMAT) combined with low temperature annealing revealed an improvement in corrosion resistance attributed to surface nanocrystallization which improved the passivation ability.⁹⁷⁾ In this sense, although the surface modification reached using SMAT has beneficial effects, the corrosion behavior could be influenced because of the higher surface roughness, high density of defects and dislocations and strained induced martensite.⁹⁸⁾

Zhao et al.⁹⁹⁾ studied AISI 304 ultrafine grain steel produced through cryogenic rolling. The corrosion resistance of the ultrafine-grained samples increased as the annealing temperature increased from 700°C to 900°C, presenting lower I_corr, which is a criterion to evaluate corrosion resistance.¹⁰⁰⁾ The results showed that the Cr-rich carbide precipitates formed during the process affect the stability of the austenite and lead to the formation of Cr-depleted regions around the precipitates. For AISI 304L processed using SMAT, the passivation current lowers after SMAT indicating a better surface protection ability than the untreated surface.¹⁰¹⁾

Li et al. investigated the effect of deformation-induced martensite on the corrosion behavior and the interaction between cavitation erosion (CE) and corrosion of 304 stainless steel. They found that martensite promoted the pitting sensitivity of the steel and decreased the stability of passive films. In addition, an accelerated effect of corrosion to CE had an essential effect on material damage.¹⁰²⁾ In other work, the susceptibility to stress corrosion cracking (SCC) of 304L steel processed through surface mechanical attrition treatment (SMAT) was studied, showing that the SMAT specimen was mainly composed of strain-induced martensite that contributes to forming or accumulating crack nucleation sites, which are the spots where the SCC initiates preferentially.¹⁰³⁾ In this sense, the strain-induced martensite formed during SPD process for austenitic stainless steels could deteriorate corrosion resistance.¹⁰⁴⁾

Zhang et al. reported high-nitrogen stainless steel (HNS) processed using Friction Stir Processing (FSP). Ultra-high strength of up to 1.7 GPa and excellent corrosion resistance was reported, mainly attributed to the ultra-fine-grained uniform microstructure obtained, which improved the repassivation of HNS. The passive film formed on the ultrafine-grained HNS showed high resistance to nucleation and pit growth. It was confirmed that ultra-grain refinement is an effective method to improve the corrosion resistance of HNS without sacrificing strength. The surface pitting morphologies obtained by the authors after immersion in a FeCl₃ solution for 10 and 24 h are shown in Fig. 3. A high pitting density was observed on the base metal surface after 10 h of immersion (Fig. 3(a)). However, no large pits could be detected on the surface of the FSP sample (Fig. 3(b)). After immersion for 24 h, the base metal was severely corroded, showing large pits with a diameter of more than 150 µm (Fig. 3(c)). No large pits were found in the FSP sample (Fig. 3(d)), revealing the increase in the resistance to pitting formation in the treated material.¹⁰⁵⁾

Fig. 3

Pitting morphologies of the HNS samples immersed in a FeCl₃ solution: (a) Base metal after immersion for 10 h, (b) FSP sample after immersion for 10 h, (c) Base metal after immersion for 24 h and (d) FSP sample after immersion for 24 h.¹⁰⁵⁾

According to the previously exposed, the corrosion behavior of stainless steels subjected to grain refinement using SPD is not consistent, because the effects of grain size grain on corrosion resistance are very complicated, as demonstrated in Table 1, which shows the changes in corrosion resistance of several stainless steels with grain refinement. The main difficulties obtaining UFG steels of consistently high corrosion resistance have been attributed to the following factors. The first is the density of defects. Segregation of alloying elements, phase transformation, and the formation of inclusions, among others, affect passive layer properties with different defect densities. In addition, high-energy zones with many dislocations would result in a high pitting rate.^106,107) The second is the grain size distribution. With the same average grain size, the microstructure with uniform grains showed good corrosion resistance in a passivating environment. A non-uniform grain microstructure may appear in SPD processes at non-uniform deformation and temperature, affecting all microstructure dependent properties. In addition, grain boundary interactions with alloying elements and impurities influence steel corrosion resistance.^105,108,109) In addition, the corrosion resistance depends on the passivation capability of the steel in active or passive aggressive media. In active solutions, grain refinement deteriorates or improves corrosion resistance depending on the solubility on the corrosion products on the surface, whereas in passive solutions grain refinement is beneficial to the formation of a protective passive film.¹¹⁰⁾

Table 1 Effect of grain size on corrosion resistance in previous studies.

3.3 Tool steels

Although there are some works dedicated to study the grain refinement and properties of tool steels processed by SPD,^14,62–64) no studies were found for corrosion behavior in these steels. In many applications, tool steels are coated with transition metal carbides to improve corrosion resistance. Some authors report the improvement in the corrosion resistance of AISI D2^111–117) and AISI H13¹¹⁵⁾ tool steel with the production of a layer of chromium niobium carbide on the steel surface, and other works have reported that for tool steels the corrosion behavior could be more influenced by its phase composition that the nanocrystalline structure.¹¹⁸⁾

4. Conclusion

This paper provides a comprehensive review on the corrosion behavior of steels processed using Severe Plastic Deformation Techniques. The steels were categorized into three groups according to their composition. The microstructural changes when processing these steels using different SPD techniques were presented, mainly those related to phase changes. For the three types of steel, phase transformations have been reported when processing using SPD, which have direct influence on corrosion behavior.

For carbon, alloyed and stainless steels, the formation of a passive film on the steel surface and its stability plays an important role on the corrosion behavior because it acts as a protective layer against corrosion. However, this passive film is influenced by the density of defects, including grain boundaries density, dislocation density, segregation of alloying elements, phase transformations, formation of inclusions and Cr content among others, as well as grain size distribution.

The strain induced martensite affects the localized corrosion resistance and therefore the steels could degrade through different corrosion mechanisms with time. This means that real-time monitoring in different environments need to be conducted.

In this sense, the resulting corrosion behavior of steels could be controlled by choosing the right process and using the correct parameters during treatment, according to the initial state of the steel. However, the overall effect of the steel microstructure on corrosion behavior should be understood.

ACKNOWLEDGMENT

This work was supported by Universidad Militar Nueva Granada, Colombia.

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