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Microstructure evolution and grain refinement mechanism of 316LN steel

  • Li Zhang EMAIL logo , Jie Ren , Zhichao Zheng , Lanfang Guan EMAIL logo , Chengzhi Liu , Yanlian Liu , Shengwei Cheng , Zexing Su and Fei Yang
Published/Copyright: November 5, 2024
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High Temperature Materials and Processes
From the journal High Temperature Materials and Processes Volume 43 Issue 1

Abstract

The hot compression behavior of 316LN stainless steel for the supporting system in a magnet confinement fusion reactor was isothermally compressed at 1,050℃ and 0.1 s−1. Electron backscatter diffraction was used to study the microstructure and texture evolution during the deformation process. The results showed that the necklace structure is eventually formed by increasing compression strain due to dynamic recrystallization (DRX). The proportion of low-angle grain boundaries first increases and then decreases. The dominant DRX mechanism of 316LN is discontinuous DRX, which is characterized by the grain boundary bulging. Besides, twinning is found to be induced to accommodate the plastic strain, helping the development of DRX.

Keywords: hot compression; texture evolution; dynamic recrystallization; twinning

1 Introduction

The conflict between growing global energy demand and climate change is a grand challenge that requires the development of clean, safe, and sustainable energy technology. Nuclear power based on fusion reaction has been widely accepted as a promising option. Scientists have been trying to figure out how to produce this energy through various experiments for decades. Finally, it came up to Tokamak’s device, a chamber using a powerful magnetic field to contain the hot plasma [1]. Gravity support (GS) is a key component supporting the Tokamak magnet coil. Due to the harsh working environment (extreme temperature, large stress, neutron irradiation, etc.), GS will be subjected to extreme loads, including deadweight, huge electromagnetic force, and thermal stress [2,3]. Therefore, the support material should have excellent strength, considerable toughness and plasticity, and good radiation resistance.

316LN austenitic stainless steel with high nitrogen content (0.12–0.22 wt%), which has been used in ITER, EAST, and KSTAR nuclear fusion devices, has been proven to be an ideal candidate for support systems [4]. Before manufacturing the GS component, a general understanding of the processing character of the 316LN is of critical importance. Thus, it is necessary to study the thermal deformation behavior of 316LN and analyze its mechanism of microstructure refinement.

In recent years, the hot deformation behavior and dynamic recrystallization (DRX) mechanism of 316LN have been studied. Chen et al. [5] developed a multi-layer cellular automaton model to describe the deformation behavior of 316L and its DRX nucleation mechanism. Liu and Chen [6] found that during the thermomechanical processing of 316LN steel, zigzag grain boundary bulging appears due to twinning. Kumar et al. [7] analyzed the effect of N content in 316LN stainless steel on DRX behavior. They found that high nitrogen content was conducive to early nucleation of DRX at low temperatures. Though many studies focused on the influence of deformation parameters (temperature and strain rate) on DRX behavior, there are few reports on the microstructure evolution and DRX mechanism during the thermomechanical deformation process. Therefore, in this research work, the microstructure evolution and grain refinement mechanism of 316LN steel used in the GS of a Tokamak were systematically studied.

2 Materials and methods

The experimental material used in this study is 316LN, and its chemical composition is shown in Table 1.

Table 1

Chemical composition of 316LN ultra-low carbon nitrogen controlled austenitic steel (wt%)

C Si Mn Cr Ni Mo Cu N Fe
0.02 0.5 0.7 18.0 12.0 3.0 0.65 0.6 Bal.

Cylindrical specimens of Φ8 mm × 12 mm were machined from a 316LN block. The specimens were then iso-thermally compressed on the Gleeble-3500 simulation test machine. The experimental parameters were as follows: heating rate of 10℃·s−1, compression temperature of 1,050℃, dwelling time of 120 s, and strain rate of 0.1 s−1. The degree of deformation was defined as 5, 10, 20, 40, and 60%, respectively. After compression, the specimens were quickly water-cooled to retain the high-temperature deformation structure. After the compression, the sample was cut along the longitudinal section by a wire-cutting machine, and the middle (large deformation) area was taken for microstructure analysis.

Optical microscopic observation was carried out along the longitudinal section after mechanical polishing and etching. Electron backscatter diffraction (EBSD) samples were prepared by electrolytic polishing with a mixture solution of 20 vol% perchloric acid alcohol solution. Siron 200 field emission scanning electron microscope equipped with the EBSD system of Oxford instrument was used for EBSD observation, and then HKL Channel5 software was used for data processing [8].

3 Results

3.1 Initial microstructure of 316LN

Figure 1a shows an EBSD image of the initial microstructure of 316LN, mainly composed of equiaxed grains and many annealing twins with straight boundaries. The average grain size statistically measured is 45.6 μm. The crystal orientation of 316LN steel is shown in Figure 2b, showing randomly oriented grains. Figure 2c shows the angle distribution of grain boundaries of the initial grains, with the proportion of high-angle grain boundaries (HAGBs) and low-angle grain boundaries (LAGBs) accounting for 57.2 and 42.8%, respectively.

Figure 1 Microstructure of the 316LN steel specimen before hot deformation: (a) orientation image microscopy map; (b) inverse pole figure; and (c) misorientation distribution map.
Figure 1

Microstructure of the 316LN steel specimen before hot deformation: (a) orientation image microscopy map; (b) inverse pole figure; and (c) misorientation distribution map.

Figure 2 Metallographic microstructure maps of 316LN compressed at (a) 0.05; (b) 0.1; (c) 0.22; (d) 0.4; and (e) 0.6 and (f) stress–strain curve.
Figure 2

Metallographic microstructure maps of 316LN compressed at (a) 0.05; (b) 0.1; (c) 0.22; (d) 0.4; and (e) 0.6 and (f) stress–strain curve.

3.2 Microstructure evolution of 316LN during processing

Figure 2(a–e) shows the metallographic microstructure maps of 316LN compressed at 1,050℃ and 0.1 s−1. Figure 2f shows the true stress–strain curve of hot deformation, where the degree of deformation at the five state points a–e corresponds to Figure 2(a–e), respectively. Before the compression strain reaches 0.05, few grain changes occur compared to the initial structure. When the compression strain reaches 0.1, some grain boundaries are bulging. At the strain of 0.22, the grains are compressed to a greater extent, elongated along the direction perpendicular to the compression axis, and the grain boundary bulge is more prominent. As the strain increases, fine recrystallized grains appear at some grain boundaries, and the number of twins decreases significantly. When the strain increases to 0.9, more new recrystallized grains were formed along the original grain boundaries, but the formed recrystallized grains were smaller in size and mixed with coarse deformed grains to form a typical “necklace structure.”

Figure 3(a–e) shows the grain boundary maps of 316LN steel compressed to different degrees at 1,050°C and 0.1 s−1, in which LAGBs, HAGBs, and twin boundaries (TBs) are represented in black, green, and red, respectively. The proportion of different types of grain boundaries with the increase in strain is shown in Figure 3f. It can be seen that the proportion of LAGBs first increases and then decreases with the increase in strain. Since at low strain, the energy storage is insufficient to induce DRX. Once DRX occurs, the nucleation and growth of DRX grains continuously consume dislocations, thus reducing the proportion of LAGBs. The trends of HAGBs and TBs are opposite to those of LAGBs, and the increase of HAGBs is due to the formation of new DRX grains at the late stage of hoter deformation, so it can be inferred that there is also some connection between TBs and DRX process.

Figure 3 Grain boundary maps of the 316LN steel at the strains of (a) 0.05; (b) 0.1; (c) 0.22; (d) 0.51; and (e) 0.9 (under 1,050°C and 0.1 s−1) and (f) variations of different kinds of GBs.
Figure 3

Grain boundary maps of the 316LN steel at the strains of (a) 0.05; (b) 0.1; (c) 0.22; (d) 0.51; and (e) 0.9 (under 1,050°C and 0.1 s−1) and (f) variations of different kinds of GBs.

Figure 4(a–e) shows the deformation-recrystallization (DefRex) maps of 316LN austenitic stainless steel after hot deformation at different strain levels (1,050°C, 0.1 s−1), in which deformed, substructured, and recrystallized grains are shown in grey, yellow, and blue, respectively, and the percentages of different types of grains are shown as histograms in Figure 4f. Obviously, when the strain is small, the energy storage of the deformation within the material is less and it is difficult to induce the occurrence of DRX as shown in Figure 4(a and b). At this time, the existence of the DRX region can hardly be observed. As the strain increases, the degree of deformation of the structure increases, and the energy storage in the material continues to accumulate. When the strain is increased to 0.51, the region with a high degree of local deformation in the material has enough stored energy to drive DRX, and the recrystallization grains begin to nucleate and grow at the original grain boundaries, as shown in Figure 4d. At this point, the proportion of recrystallized grains is %. When the strain variable reaches 0.9, to resist greater deformation resistance, DRX starts to occur frequently and the recrystallization proportion of DRX grains is further increased with small and continuous distribution around the deformation area.

Figure 4 DefRex maps of 316LN austenitic stainless steel after hot compression at different strains (1,050℃, 0.1 s−1): (a) ε = 0.05; (b) ε = 0.1; (c) ε = 0.22; (d) ε = 0.51; and (e) ε = 0.9 and (f) histogram of grain proportion of different types.
Figure 4

DefRex maps of 316LN austenitic stainless steel after hot compression at different strains (1,050℃, 0.1 s−1): (a) ε = 0.05; (b) ε = 0.1; (c) ε = 0.22; (d) ε = 0.51; and (e) ε = 0.9 and (f) histogram of grain proportion of different types.

The changes in DRX area fraction and average grain size with strain are shown in Figure 5, and the results indicate that DRX has a great influence on grain size. The average grain size of the sample decreases with the increase in DRX proportion, and the faster the increase in DRX proportion, the faster the grain size reduction rate, indicating that DRX is the main mechanism of grain refinement. When the true strain increases to 0.9, the average grain size decreases from 41.2 μm to about 5 μm, and the grain is further refined.

Figure 5 The relationship between the degree of recrystallization and the average grain size.
Figure 5

The relationship between the degree of recrystallization and the average grain size.

4 Discussion

4.1 Recrystallization mechanism

We selected two typical specimens to reveal the DRX mechanism of 316LN during iso-thermal compression. It can be observed from Figure 6a that the original grain boundaries bulge and part of the grain boundaries are serrated, which is a typical sign of discontinuous DRX bulging mechanism [9], mainly driven by the energy generated by the dislocation density difference on both sides of adjacent grain boundaries, commonly known as the strain-induced grain boundary migration mechanism [10]. When ε = 0.9, the deformation energy storage under significant strain increases, and the grain boundary bulge is more pronounced, as shown in Figure 6b, where both the grain boundaries are serrated, and the grain boundaries are surrounded by dislocation-free recrystallized grains. It is well known that the process of DRX includes apparent nucleation and growth, and the grain boundary serves as a site to accommodate the accumulation of dislocations, resulting in the primordial HAGBs and its triple junction preferentially becoming the nucleation site of DRX.

Figure 6 Local orientation image microscopy maps at the strains of (a) 0.22 and (b) 0.9 and changes of misorientation angle along the lines marked in black: (c) AB; (d) EF; (e) CD; and (f) GH.
Figure 6

Local orientation image microscopy maps at the strains of (a) 0.22 and (b) 0.9 and changes of misorientation angle along the lines marked in black: (c) AB; (d) EF; (e) CD; and (f) GH.

The orientation deviation of grains during recrystallization was calculated along the black lines in Figure 6a and b, as shown in Figure 6(c–f). The blue curve represents the local orientation deviation (point-to-point), and the red curve represents the cumulative orientation deviation (point-to-origin). The local orientation deviation along the original grain boundary and in the crystal is less than 3°, and the cumulative orientation deviation is less than 15°. However, the cumulative orientation of both of them shows a significant increase in the orientation difference gradient at 80 μm; this is a result of the progressive subcrystalline rotation of the continuous DRX mechanism [11]. When the deformation degree increases, the local orientation deviation at grain boundaries and within grains fluctuates to different degrees, with the deviation angle exceeding 5° and the cumulative orientation deviation easily exceeding 15°, as shown in Figure 6d and f. This indicates that HAGBs have formed between the original grain and its internal substructure at this stage, a consequence of the continuous rotation of the substructure caused by the activation of the sliding system. The degree of progressive rotation of the subcrystal has been relatively developed.

4.2 Twinning assisted DRX

A coincident site lattice (CSL) grain boundary is a special interface that can meet the requirements of coincidence site lattice by sharing some lattice points and affecting the material properties and is characterized by ∑. The TB, namely the ∑3 coherent TB, is an important part of the low ∑-CSL ∑ ≤ 29 grain boundary and plays an important role in distinguishing recrystallized grains from deformed grains. Figure 7 clearly shows the role of twinning in the separation and nucleation of the DRX bulge, while other low CSL boundaries are also involved in the formation of new HAGBs and the separation from the parent crystal. In DRX, the twin at the interface will essentially change the misorientation, thus providing additional boundary energy for migration and growth, increasing the mobility of its moving boundary, and speeding up the DRX process. This twinning at the interface allows DRX volumes to grow perpendicular to the interface and in parallel directions [12,13,14]. In addition, the presence of twins helps the crystal to change from hard orientation to soft orientation, and the TB also provides more favorable places for recrystallization nucleation, further promoting the occurrence of DRX.

Figure 7 Local grain boundaries of samples at typical strain: (a) 0.22 and (b) 0.9.
Figure 7

Local grain boundaries of samples at typical strain: (a) 0.22 and (b) 0.9.

5 Conclusions

The microstructure evolution of 316LN steel at 1,050℃ and 0.1 s−1 was studied by hot compression test. Some important conclusions can be made as follows:

  1. The DRX process consumes deformed substructures, resulting in a gradual reduction of LAGBs and an increase in HAGBs.

  2. DDRX, characterized by zigzag grain boundary bulging nucleation, is the primary grain refinement mechanism of the steel grades studied.

  3. Twinning is an indispensable auxiliary deformation mechanism under experimental conditions, which accelerates the separation of the DRX grain boundary from the parent crystal and greatly promotes the DRX process.

# Jie Ren contributed equally to this work and should be considered as the co-first author.

Acknowledgements

The present study was based on North University of China, and we thank the university and all authors for their assistance.

  1. Funding information: The present study was sponsored by the Fundamental Research Program of Shanxi Province under Grant Nos. 202203021212117 and 202303021212181; the Science and Technology Innovation Project of Colleges and Universities in Shanxi Province under Grant Nos. 2020L0311 and 2020L0320; and Young Elite Scientists Sponsorship Program by CAST under Grant No. 2023QNRC001.

  2. Author contributions: Li Zhang: writing – review & editing; Jie Ren: writing – original draft, Formal analysis; Zhichao Zheng: experimental preparation, methodology; Lanfang Guan: methodology, formal analysis; Chengzhi Liu: resources, supervision; Yanlian Liu: project administration; Shengwei Chen: resources; Zexing Su: visualization; and Fei Yang: formal analysis.

  3. Conflict of interest: The authors state no conflict of interest.

  4. Data availability statement: The data presented in this study are available on request from the corresponding author.

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Received: 2024-04-16
Revised: 2024-05-27
Accepted: 2024-05-29
Published Online: 2024-11-05

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/htmp-2024-0038
Keywords for this article
hot compression; texture evolution; dynamic recrystallization; twinning
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  31. Research on the influence of cemented carbide micro-textured structure on tribological properties
  32. Performance evaluation of fly ash-lime-gypsum-quarry dust (FALGQ) bricks for sustainable construction
  33. First-principles study on the interfacial interactions between h-BN and Si3N4
  34. Analysis of carbon emission reduction capacity of hydrogen-rich oxygen blast furnace based on renewable energy hydrogen production
  35. Just-in-time updated DBN BOF steel-making soft sensor model based on dense connectivity of key features
  36. Effect of tempering temperature on the microstructure and mechanical properties of Q125 shale gas casing steel
  37. Review Articles
  38. A review of emerging trends in Laves phase research: Bibliometric analysis and visualization
  39. Effect of bottom stirring on bath mixing and transfer behavior during scrap melting in BOF steelmaking: A review
  40. High-temperature antioxidant silicate coating of low-density Nb–Ti–Al alloy: A review
  41. Communications
  42. Experimental investigation on the deterioration of the physical and mechanical properties of autoclaved aerated concrete at elevated temperatures
  43. Damage evaluation of the austenitic heat-resistance steel subjected to creep by using Kikuchi pattern parameters
  44. Topical Issue on Focus of Hot Deformation of Metaland High Entropy Alloys - Part II
  45. Synthesis of aluminium (Al) and alumina (Al2O3)-based graded material by gravity casting
  46. Experimental investigation into machining performance of magnesium alloy AZ91D under dry, minimum quantity lubrication, and nano minimum quantity lubrication environments
  47. Numerical simulation of temperature distribution and residual stress in TIG welding of stainless-steel single-pass flange butt joint using finite element analysis
  48. Special Issue on A Deep Dive into Machining and Welding Advancements - Part I
  49. Electro-thermal performance evaluation of a prismatic battery pack for an electric vehicle
  50. Experimental analysis and optimization of machining parameters for Nitinol alloy: A Taguchi and multi-attribute decision-making approach
  51. Experimental and numerical analysis of temperature distributions in SA 387 pressure vessel steel during submerged arc welding
  52. Optimization of process parameters in plasma arc cutting of commercial-grade aluminium plate
  53. Multi-response optimization of friction stir welding using fuzzy-grey system
  54. Mechanical and micro-structural studies of pulsed and constant current TIG weldments of super duplex stainless steels and Austenitic stainless steels
  55. Stretch-forming characteristics of austenitic material stainless steel 304 at hot working temperatures
  56. Work hardening and X-ray diffraction studies on ASS 304 at high temperatures
  57. Study of phase equilibrium of refractory high-entropy alloys using the atomic size difference concept for turbine blade applications
  58. A novel intelligent tool wear monitoring system in ball end milling of Ti6Al4V alloy using artificial neural network
  59. A hybrid approach for the machinability analysis of Incoloy 825 using the entropy-MOORA method
  60. Special Issue on Recent Developments in 3D Printed Carbon Materials - Part II
  61. Innovations for sustainable chemical manufacturing and waste minimization through green production practices
  62. Topical Issue on Conference on Materials, Manufacturing Processes and Devices - Part I
  63. Characterization of Co–Ni–TiO2 coatings prepared by combined sol-enhanced and pulse current electrodeposition methods
  64. Hot deformation behaviors and microstructure characteristics of Cr–Mo–Ni–V steel with a banded structure
  65. Effects of normalizing and tempering temperature on the bainite microstructure and properties of low alloy fire-resistant steel bars
  66. Dynamic evolution of residual stress upon manufacturing Al-based diesel engine diaphragm
  67. Study on impact resistance of steel fiber reinforced concrete after exposure to fire
  68. Bonding behaviour between steel fibre and concrete matrix after experiencing elevated temperature at various loading rates
  69. Diffusion law of sulfate ions in coral aggregate seawater concrete in the marine environment
  70. Microstructure evolution and grain refinement mechanism of 316LN steel
  71. Investigation of the interface and physical properties of a Kovar alloy/Cu composite wire processed by multi-pass drawing
  72. The investigation of peritectic solidification of high nitrogen stainless steels by in-situ observation
  73. Microstructure and mechanical properties of submerged arc welded medium-thickness Q690qE high-strength steel plate joints
  74. Experimental study on the effect of the riveting process on the bending resistance of beams composed of galvanized Q235 steel
  75. Density functional theory study of Mg–Ho intermetallic phases
  76. Investigation of electrical properties and PTCR effect in double-donor doping BaTiO3 lead-free ceramics
  77. Special Issue on Thermal Management and Heat Transfer
  78. On the thermal performance of a three-dimensional cross-ternary hybrid nanofluid over a wedge using a Bayesian regularization neural network approach
  79. Time dependent model to analyze the magnetic refrigeration performance of gadolinium near the room temperature
  80. Heat transfer characteristics in a non-Newtonian (Williamson) hybrid nanofluid with Hall and convective boundary effects
  81. Computational role of homogeneous–heterogeneous chemical reactions and a mixed convective ternary hybrid nanofluid in a vertical porous microchannel
  82. Thermal conductivity evaluation of magnetized non-Newtonian nanofluid and dusty particles with thermal radiation
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