Effect of induction heat treatment on microstructure, mechanical and corrosion properties of stainless steel 308 L fabricated using wire arc additive manufacturing | Scientific Reports

Scientific Reports volume 14, Article number: 26089 (2024) Cite this article Metrics details Induction solution heat treatment can change the mechanical characteristics and corrosion resistance

Scientific Reports volume 14, Article number: 26089 (2024) Cite this article

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Induction solution heat treatment can change the mechanical characteristics and corrosion resistance properties of 308 L manufactured via wire arc additive manufacturing (WAAM). Moreover, compare with traditional heat treatment methods, this method can reduce heat treatment time and achieve in-situ local heat treatment. In this paper, in-situ induction heat treatment at 1100 °C for 2, 4, and 6 min were applied on 308 L thin-walled parts produced by WAAM. The result show that ferrite and austenite phase proportions were changed after induction solution heat treatment. Heat treatment at 1100 °C effectively reduced the δ-Fe and σ-Fe content, resulting in a slight decrease in UTS and microhardness, while YS and EL have a certain degree of increase. σ-Fe exhibits a more pronounced strengthening effect than austenite, albeit at the potential expense of steel’s elasticity. At the same time, induction heat treatment alters the ferrite to austenite ratio, which also enhances the anti-corrosion properties of the stainless steel. However, the presence of σ-Fe will cause a worsening of the corrosion resistance of the steel. In addition, as the heat treatment progresses, the ferrite’s microstructure in the deposition direction undergoes a significant transformation, changing from continuous dendrites to a few equiaxed grains.

Wire arc additive manufacturing (WAAM) can enable the direct fabrication or restoration of metal parts1. Compared with conventional manufacturing methods like casting and forging, WAAM offers technical and economic advantages such as high material utilization rate, low manufacturing cost, and manufacturing of complex structural parts2. The technique uses an electric arc to melt the wire and stack the metal layer by layer to obtain a production part, guided by a layered approach from a computer-aided design model3. However, due to the extensive heat input, high-temperature gradient, and complex thermal history in the manufacturing process4, the obtained part materials are quite different from those obtained by traditional manufacturing methods in terms of microstructure and mechanical properties, and uncontrollable changes in material properties will have an impact on the performance of the parts5.

Austenitic stainless steel is a prevalent metallic material extensively employed in contemporary industries such as shipbuilding, aerospace, and nuclear reactors because of its favorable corrosion resistance, mechanical properties, and processibility6,7. Austenitic stainless steel is mainly composed of austenite, ferrite, and minor quantity of carbide, among which ferrite can be divided into δ-Fe and σ-Fe. δ-Fe is a high-temperature ferrite produced during solid solution phase transformation, and σ-Fe is generated from δ-Fe when the material is exposed to 450 °C~850 °C for a long time8,9. Studies have shown that in austenitic stainless steel obtained by welding or other processes, the σ phase in ferrite can play a specific role in strengthening10. However, at the same time, due to its hard and brittle characteristics, if it exists in large amounts, it will reduce the plasticity and corrosion resistance of the steel11. Chen studied the microstructure of laser welded NiTi/304 stainless steel joints using Ni as filler material. Intermetallic compounds such as Ni3Ti are formed in welded joints, and these compounds may cause uneven microstructure distribution during the welding process12. Lin proposed to use the healing mechanism of voids in cold rolled M50 bearing steel for aero-engines under electric shock treatment was studied. The dynamic behavior and healing process of voids during electric shock treatment were revealed through experimental and simulation studies13. Both of above studies are for Ti/Ni alloy. Shao proposed to use situ nanoindentation technique to improve the cracks defects caused by the ultrasonic pulse frequency tungsten inert gas welding14.Zhang investigated the interface morphology, phase composition, and mechanical properties of joints fabricated using the nano-Sn-3.0Ag-0.5Cu soldering paste and MHH technique with varying exposure times15. According to these literatures, it can be found that the research on the microstructure and mechanical properties of Stainless Steel 308 L formed by WAAM process is rarely mentioned.

The temperature history during the WAAM process is complex and uncontrollable, and there are many phase transition processes. It is easy to cause more ferrite phases to exist16. In addition, the microstructure of stainless-steel shows that σ-Fe appears in a dendritic form, with grain growth in the direction opposite to the direction of maximum cooling, which is usually consistent with the deposition direction17. The dendrite structure is also different at different deposition positions, leading to disordered microstructure distribution and poor homogeneity, differences in mechanical properties at different locations, and poor homogeneity of part performance18.

Li et al. studied the high-temperature fatigue behavior of AM Ti-6Al-4 V alloy processed by HIP. They conducted fatigue tests at 200 °C and 400 °C to improved fatigue life of materials19. Zhang et al. studied the electrochemical behavior and anti-corrosion passivation properties of TiZrHfNb multi-principal alloy20. Xu et al. studied the corrosion resistance enhancement mechanism of Ni-8Al alloy by high-speed laser coating preparation technology21. Li et al. studied the characteristics of cold sprayed copper coatings deposited on 6061 T6 aluminum alloy substrates under different gas temperatures and pressures and explored the effects of subsequent heat treatment on the microstructure and mechanical properties of the copper coatings22. It can be seen from these literatures that the mechanical properties and environmental resistance of materials can be significantly improved by precisely controlling the microstructure of materials. For example, through heat treatment and coating technology, the fatigue resistance and ablation resistance of materials can be improved. These studies provide important guidance for the design and processing of materials, especially for applications in aerospace, energy, and electrical engineering.

In order to improve the material properties of WAAM austenitic stainless steel, it is necessary to take specific performance optimization methods. Heat treatment is a common material modification method, and some researchers have applied it to WAAM austenitic stainless steel. Chen et al.23. conducted solution heat treatment of WAAM 316 L stainless steel and found that water quenching after heat treatment at a temperature of 1100 °C~1200 °C could eliminate the ferrite in the steel, reduces strength, and increases ductility and corrosion resistance. This heat treatment method can also eliminate the effect of work hardening, leading to a reduction in the material’s surface hardness. In addition, regulating both the temperature and duration of the heat treatment process is essential to prevent sensitization and preserve corrosion resistance. Rodrigues et al.24 established a synchrotron X-ray diffraction analysis method to measure ferrite and austenite in the induction heat treatment of austenitic stainless steel. The higher dissolution temperature can effectively dissolve δ-ferrite dendrites distributed in the austenite matrix. Induction solution heat treatment can change the mechanical characteristics and corrosion resistance properties of 308 L manufactured via wire arc additive manufacturing (WAAM). Moreover, compare with traditional heat treatment methods, this method can reduce heat treatment time and achieve in-situ local heat treatment. However, the researchers did not describe the changes in the material properties of the steel after induction heat treatment, such as mechanical and corrosion resistance properties.

In the present study, induction heat treatment was performed on the 308 L thin-walled parts fabricated by WAAM. This work is devoted to the systematic study of the effects of induction heat treatment at different heating time on the phase transformation and microstructure evolution of the parts using optical microscope (OM), scanning electron microscopy (SEM), and X-ray Diffraction (XRD). Moreover, tensile testing, microhardness testing, and electrochemical testing were conducted to deeply analyze the strengthening mechanism of mechanical properties and corrosion resistance. It was found that the mechanical properties and corrosion resistance were improved after induction solution heat treatment due to the reduction of σ-Fe and the transformation of microstructure.

This study uses 100 mm × 150 mm × 4 mm thin-walled parts made by WAAM using 1.2 mm diameter 308 L stainless steel wire. The chemical compositions of the 308 L stainless steel wire and process parameters are listed in Tables 1 and 2, respectively. The specific manufacturing equipment process are shown in Fig. 1, among which the six DOF manipulator can realize the movement of parts between the arc additive manufacturing station and the induction heating station.

The WAAM equipment system.

In-situ induction heat treatment was performed on thin-walled parts made by WAAM, utilizing the principles of electromagnetic induction and the current skin effect. The heat treatment system consists of two parts: induction heating power supply (which is made by Polaris E-Tek Shenzhen, Model DIH-40) and the infrared thermometer (which is made by Shaanxi RG Automatic instrument co., Ltd, Mode ST201-A). The infrared thermometer can give thermo-feedback to heating power supply to control the system’s temperature. The induction heat treatment system was shown in Fig. 2, with a temperature control accuracy of ± 1%, as same as that of the infrared thermometer. In the heat treatment experiment, three control groups were set as with the holding time as the variable, heat treatment was performed at 1100 ℃ for 2 min, 4 min and 6 min, using water as the quenching cooling medium, as listed in Table 3.

Induction heating equipment system.

Metallographic specimens were prepared through wire-electrode cutting from both as-deposited and heat-treated parts, and then a series of polishing steps were performed on specimens involving 180#, 240#, 800#, 1200#, 1500#, and 2000# grit sandpaper, and W0.5 grit polishing agent in turn for grinding and polishing. Subsequently, the specimens were etched with a solution comprising 20 ml of HCl, 20 ml of H2O, and 4 g of CuSO4. The microstructural characterization of the 308 L fabricated using WAAM was conducted utilizing the ZEISS optical microscope (OM) and the Gemini-SEM 300 scanning electron microscope (SEM). To ensure the precision of the results, the volume fraction (vol%) values of austenite and ferrite phases in 308 L specimens were determined from metallographic photographs using Image-Pro Plus software under deposition and heat treatment conditions. Additionally, these values were cross-verified with data obtained through X-ray Diffraction (XRD) analysis using the quantitative phase analysis module of Jade software.

Tensile testing was conducted according to the ASTM E8 standard using the SAS Test CMT5205 electronic universal testing machine. Tensile testing was carried out at room temperature with the crosshead speed set at 0.5 mm/minute and the strain during the test was recorded by an electronic tensiometer. The dimension of the plate specimen prepared for tensile tests was 25 mm in gauge length, 100 mm in total length and 4 mm in thickness. The direction of tensile specimens was parallel to the deposition direction as depicted in Fig. 3. To mitigate measurement discrepancies, at least three samples were tested under identical conditions and their average values were calculated. Cut the hardness test sample at the same height in the center of each part. Microhardness was measured with an MH-5 Vickers hardness tester. The test load was set as 200 g and the pressure holding time was set as 10 s.

Schematic diagram of tensile specimens.

Samples used for the electrochemical testing were 5 × 5 × 3 mm3 in size and put in a 0.5 cm2 sample support box as a working electrode. The surface of each sample was firstly ground to 2000#, followed by a polishing step employing 0.5 μm diamond paste. Electrochemical tests were performed using the Versa STAT 3 electrochemical workstation with a corrosion solution of 3.5wt % NaCl solution at room temperature (25 ℃). A three-electrode system consisting of the counter electrode, the reference electrode, and the working electrode was used for the electrochemical testing. For these experiments, the counter electrode was composed of platinum foil, while the reference electrode used a saturated calomel electrode (SCE). In order to establish steady-state conditions, firstly record the open circuit potential (Eo) for 40 min. Set the sweep rate of dynamic polarization curve test to 30 mV/min, starting at 50 mV below the steady open circuit potential and ending when the current density surpassed 10− 4 A/cm2. In the polarization curve, the pitting potential (Ep) is the potential at which the current density increased significantly. According to the polarization curves of samples, the corrosion current density (icorr) was determined by using Tafel extrapolation method.

In as-deposited 308 L stainless steel, the ferrite exhibits a dendritic morphology within the austenite matrix. The dendrites are more continuous in the deposition direction, and the growth direction is consistent with the deposition direction. The morphology is more dispersed in the printing direction, as can be seen from Fig. 4. After induction heat treatment at 1100 °C, the ferrite will gradually dissolve in the austenite matrix. As shown in Fig. 5, after 2 min of solid solution treatment, ferrite appears as broken dendrites are. At 4 min, it takes on a spheroid, while at 6 min, it appears granular. As the solid solution time increases, the ferrite content gradually decreases, and its distribution in the matrix becomes more uniform. The volume fractions of ferrite and austenite in both as-deposited and heat-treated steel specimens were determined by XRD results and metallographic analysis, as shown in Fig. 6. The volume fractions of ferrite and austenite phases in the as-deposited state are about 11 vol% and 89 vol%, respectively. As listed in Table 4, there is a gradual reduction in the volume fraction of ferrite as the time of the heat treatment increases. The ferrite gradually decreases from the initial 11% to about 1%. In addition, the morphology of the grains changed from columnar grains in the as-deposited state to equiaxed ones after heat treatment.

As-deposited microstructure of 308 L fabricated using WAAM: (a) deposition direction, (b) printing direction.

Variation of metallographic in deposition direction with heat treatment time: (a) as-deposited, (b) 1100 °C/2 min, (c) 1100 °C/4 min and (d) 1100 °C/6 min.

XRD diffraction analysis composition phase ratio results: (a) as-deposited, (b) 1100 °C/2 min, (c) 1100 °C/4 min, (d) 1100 °C/6 min and (e) Jade software analysis results.

As presented in Fig. 7; Table 5, the ultimate tensile strength (UTS) and the yield strength (YS) were obtained from stress-strain curves of as-deposited and heat-treated steel specimens, while the elongation (EL) was obtained by measuring the sample after breaking. The UTS and YS of 308 L stainless steels in the as-deposited state are 576 MPa and 318 MPa, respectively. After the induction solution heat treatment at 1100 °C for 2 min, UTS decreased from 576 MPa to 554 MPa, YS increased from 318 MPa to 343 MPa, and EL increased from 44.8 to 46%. With the increase of heat treatment time, after induction solution heat treatment at 1100 °C for 4 min, UTS decreased to 534 MPa, YS increased to 336 MPa, EL increased to 48.4%; after solution heat treatment for 6 min, UTS decreased to 538 MPa, YS became 336 MPa, the EL rises to 49.6%, as shown in Table 4. Compared to the untreated sample, the UTS of the induction heat treatment sample decreased by 20%, while the YS and EL increased by 20% and 10%, respectively.

Tensile test: UTS, YS and EL variation results.

The microhardness results are shown in Fig. 8. The as-deposited hardness is 210.6 HV, and the hardness is reduced after induction heat treatment. As the heat treatment time increased, it decreased from 210.6 HV to 194.9 HV, 189.2 HV, and 173.3 HV.

The result shows that the induction solution heat treatment leads to a decrease in the strength and the hardness of WAAM 308 L stainless steel but improves its ductility.

Difference of microhardness with induction solution heat treatment.

The corrosion resistance of both as-deposited and heat-treated 308 L stainless steel specimens was investigated by potentiodynamic polarization and electrochemical impedance spectroscopy in 3.5%wt NaCl solution. The polarization curves and electrochemical parameter measurements are presented in Fig. 9; Table 5. The larger the difference between pitting potential and corrosion potential (ΔE) and the lower the corrosion current density (icorr), the slower the corrosion rate and the better the corrosion resistance. As delineated in Fig. 9; Table 6, with the time of induction solution heat treatment increasing, the icorr value gradually decreases, and the ΔE value gradually increases. It means that induction solution heat treatment is an effective means of enhancing the corrosion resistance of stainless steel. The same results are obtained by polarization impedance spectroscopy and equivalent circuit simulation, as shown in Fig. 10 and Table 7.

Open circuit potential curves and polarization curves of as-deposited and heat-treated 308 L fabricated using WAAM in 3.5%wt NaCl solution (25 °C): (a) as-deposited, (b) 1100 °C/2 min, (c) 1100 °C/4 min, (d) 1100 °C/6 min.

Electrochemical impedance spectroscopy and equivalent circuit simulation results obtained following a 40 min immersion in 3.5%wt NaCl solution: (a) Nyquist diagram, (b) equivalent circuit, (c) Bode diagram-magnitude, (d) Bode Figure - Phase Angle.

The microstructure of austenitic stainless-steel materials obtained by casting is mostly a single austenite phase, and the distribution is uniform. The austenite phase provides good plasticity and toughness, so casting is conducive to obtaining good overall plasticity and toughness. In the microstructure of cast austenitic stainless steel, a small amount of ferrite is distributed at the austenite grain boundary. Since it is less overall and distributed at the austenite grain boundary, it has little effect on the overall strength and plasticity of the casting. On the other hand, in WAAM austenitic stainless steel, due to the rapid cooling during the manufacturing process, there are more ferrites, and the distribution of ferrites is related to many factors such as the deposition path and heat dissipation conditions of the parts manufacturing process, and the distribution is messier. This may lead to the anisotropy of the material, that is, there are differences in mechanical properties in different directions. The increase of ferrite phase may increase the YS of the material but reduce plasticity. In addition, in WAAM, due to the rapid cooling and thermal cycle during the manufacturing process, more defects such as microcracks and holes may appear at the grain boundaries. These defects may become the starting point of cracks and reduce the fracture toughness of the material. Therefore, the purpose of improving the plasticity of the material can be achieved by changing the microstructure distribution of the material and improving the distribution state of ferrite through solution heat treatment.

Many researchers have done a lot of work on changing the microstructure of materials by heat treatment to improve their mechanical properties such as toughness and strength. For example, Cui used laser induced breakdown spectroscopy (LIBS) technology to classify the microstructure of steel samples with different heat treatment processes and used the matrix effect of LIBS spectrum to distinguish carbon steel samples with different microstructures25. This method does not directly change the microstructure of the material, but provides a fast and non-destructive classification method, which helps to evaluate its potential mechanical properties in material selection and quality control. Zhang studied the optimization of the microstructure of medium manganese steel by adjusting the chemical composition and heat treatment process to achieve the goals of lightweight and high strength. Special attention was paid to the problem of hydrogen embrittlement, and the capture and enrichment mechanism of hydrogen in steel was explored, as well as how to control the microstructure to reduce the impact of hydrogen embrittlement, thereby improving the toughness and plasticity of the material26. Wang proposed the preparation of face-centered cubic FeCrNi alloy by discontinuous laser scanning strategy, which increased the temperature gradient in the molten pool by reducing the thermal effect between adjacent scanning areas, thereby inhibiting the growth of cellular structure along the temperature gradient direction27. Li integrated hardness and toughness through nitrogen-induced nanocomposite structure. The researchers optimized the film’s microstructure by adjusting the nitrogen content, achieving a balance between hardness and toughness. This approach improves the material’s wear resistance and fracture resistance by precisely controlling the film’s chemical composition and microstructure28.

In our research, when the steel is heat treated at 1100 °C, the ferrite phase will transform into the austenite phase, as shown in Fig. 11, and the increase in the heating rate can significantly accelerate the austenitization rate. The preset temperature of 1100 °C can be reached in the 50 s by induction heating. Increasing the heating rate of induction heating can accelerate the rate of austenitization during heat treatment of austenitic stainless steel, thus significantly reducing the overall heat treatment time. In terms of grain morphology, the as-deposited steel exhibits a distinct dendritic structure in the deposition direction, while the grains are transformed to equiaxed by heat treatment.

Schematic diagram of the ferrite solution process: (a) microstructure after deposition, (b) microstructure after heat treatment, (c) ferrite dissolved in austenite at high temperature.

The mechanical characteristics and corrosion resistances of stainless steel are interlinked with the constituent phases and their morphology. Through the induction solution heat treatment, the decrease in the ferrite proportion resulted in a reduction of σ-Fe, which, in turn, contributed to a decline in the UTS of the stainless steel from 576 MPa to 534 MPa after heat treatment, while the YS and EL have a slight increase. The result means that ferrite plays a certain degree of strengthening effect in austenitic stainless steel, but it will adversely affect the ductility of the steel. The materials examined in this study, both before and after heat treatment, fulfill the industry’s minimum standards for forging 316 L stainless steel, as stipulated by UTS at 450 MPa, YS at 170 MPa, and EL at 40%29. For microhardness, the hardness value through heat treatment decreases gradually with the reduction of the ferrite phase and the coarsening of grains.

The potentiodynamic polarization results show a gradual reduction in the icorr of the steel and an incremental increase in the ΔE with extended heat treatment duration. These trends signify that induction solution heat treatment can effectively enhance the corrosion resistance of WAAM stainless steel. It’s a well-established fact that the formation of Cr-rich carbides along grain boundaries leads to Cr-depletion in the regions neighboring these boundaries. The σ-Fe phase, which forms and grows by consuming chromium, is notably Cr-rich. Consequently, there exists a Cr-depleted zone at the interface between the σ-Fe phase and the substrate. The passive oxide film within this chromium-depleted area is susceptible to corrosion, resulting in diminished corrosion resistance. Through the reduction of σ-Fe content, the heat-treated steel shows better corrosion resistance.

Induction heat treatment significantly reduces processing time. The high heating rate accelerates the austenitization of austenitic stainless steel, resulting in a substantial decrease in overall heat treatment duration.

Upon subjecting to heat treatment at 1100 °C, the ferrite gradually dissolves into the austenite matrix, leading to a decrease in the residual ferrite content as the time of the heat treatment progresses. The ferrite content decreases from 11% without heat treatment to 1% with 6 min induction heat treatment, which increased by 90.9%. Furthermore, the morphology of the remaining ferrite undergoes a transformation from the original dendritic to equiaxed.

The reduction of the ferrite leads to a decrease in UTS and microhardness of austenitic stainless steel after heat treatment, while a slight increase in YS and EL. After 6 min induction heat treatment, the YS and EL of 318 MPa and 44.8%, were improved to 336 MPa and 49.6%, respectively, at the expense of a small amount of part strength. It is because σ-Fe in the ferrite phase can strengthen austenitic stainless steel, but it will reduce the plasticity of the steel.

Induction solution heat treatment proves to be an effective method to improve the corrosion resistance of 308 L stainless steel. The σ-Fe phase formed in the ferrite phase results in regions depleted of chromium at their interfaces, thereby increasing the susceptibility to corrosion attack. The elimination of the ferrite phase has been shown to contribute to the effective enhancement of the corrosion resistance of austenitic stainless steels.

The datasets analyzed during the current study available from the corresponding author on reasonable request.

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This work was financially supported by The Key Research and Development Plan of Zhejiang Province (2023C01169), Natural Science Foundation of Zhejiang Province for Distinguished Young Scholars (LR22E050002), Natural Science Foundation of Zhejiang Province (LD24E050011).

The State Key Laboratory of Fluid Power and Mechatronic Systems, College of Mechanical Engineering, Zhejiang University, Hangzhou, 310027, China

Yangfan Sun, Xianglong Li, Lai Xu & Hongyao Shen

Key Laboratory of 3D Printing Process and Equipment of Zhejiang Province, College of Mechanical Engineering, Zhejiang University, Hangzhou, 310027, China

Xianglong Li, Lai Xu & Hongyao Shen

Hangzhou Wheeler General Machinery Incorporated Co., Ltd, Hangzhou, 311100, China

Yougen Liu

Zhejiang Advanced CNC Machine Tool Technology Innovation Center, Taizhou, China

Yangfan Sun

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Sun and Li wrote the main manuscript text, Xu and Liu were mainly responsible for the experiments. Shen made suggestions on the overall idea.All authors reviewed the manuscript.

Correspondence to Hongyao Shen.

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Sun, Y., Li, X., Xu, L. et al. Effect of induction heat treatment on microstructure, mechanical and corrosion properties of stainless steel 308 L fabricated using wire arc additive manufacturing. Sci Rep 14, 26089 (2024). https://doi.org/10.1038/s41598-024-75382-5

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Received: 31 July 2024

Accepted: 04 October 2024

Published: 30 October 2024

DOI: https://doi.org/10.1038/s41598-024-75382-5

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