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The investigation of peritectic solidification of high nitrogen stainless steels by in-situ observation

  • Tong Wang EMAIL logo , Sicheng Qian , Yu Wang , Yunfei Ding , Yiqiang He , Jilin Xu , Hao Xue , Wen Feng and Feng Shang
Published/Copyright: December 24, 2024
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High Temperature Materials and Processes
From the journal High Temperature Materials and Processes Volume 43 Issue 1

Abstract

High nitrogen stainless steel has wide application prospects in many fields such as aerospace, petrochemical industry, marine engineering, energy, and military. Nitrogen is added as an alloying element to replace the more expensive element, nickel, thereby reducing the cost. Since nitrogen serves as an austenite stabilizer and has a higher nickel equivalent, it can improve the corrosion resistance and other mechanical properties of the alloy, yet it could also cause porosity and cracks. As the most upstream process of material processing, the solidification process largely determines the structure and performance of the product. High temperature confocal microscope can provide in-situ observations of phase transformation in metals and alloys. Thermodynamic calculations and other research articles show that the solidification of high nitrogen stainless steel usually involves multiple phases, δ-ferrite, γ-austenite, and liquid (L). Present research utilizes a unique concentric solidification technique to manually create a solid/liquid interface for studying the coexistence of multi-phase. It was found that during the solidification process of a high nitrogen stainless steel, the γ grows along the L/δ interface (L + δ → γ), and then, the pre-formed γ through peritectic reaction grows into δ and L phase. This two-step solidification mode is a typical peritectic solidification. The intervention of N makes the solidification process of high nitrogen stainless steel extremely complicated, because N is a strong γ stabilizer, and its content dramatically affects the formation of the primary phase. The rarely reported peritectic solidification in high nitrogen stainless steel was observed, and these findings could help improve the continuous casting process of high N alloys.

Keywords: high nitrogen stainless steel; in-situ observation; concentric solidification; peritectic solidification

1 Introduction

The solidification behaviors and subsequent solid-state phase transformation, in a sense, determine the structure and properties of the material. By understanding the fundamentals of solidification behaviors we can hope to control and optimize the performance of the product at the source [1]. In high nitrogen stainless steel, various alloying elements work synergistically to give it excellent corrosion resistance and other enhanced mechanical properties. However, high contents of various alloying elements can also lead to the formation of secondary phases and intermetallic compounds due to segregation, as well as other defects. For example, in S31254 (also named as X1CrNiMoCuN20-18-7 for EN standard) super austenitic stainless steel (SASS), the segregation of nitrogen can lead to the formation of gas pores [2,3]. The participation of multiple alloying elements makes the solidification behavior of high nitrogen stainless steel very complex. However, a large number of studies have used high-end characterization equipment to investigate the structure and texture of high nitrogen stainless steel, including secondary phases, and the research on its solidification process is far from sufficient.

As an in-situ observation equipment, high temperature confocal microscope (HTCM) can conduct real-time monitoring of metals and alloys at ultra-high temperatures. It is a powerful tool for studying solidification and phase transitions. The HTCM was used to observe peritectic reactions [4–8], phase transformation sequences, and interface morphology and movement [9].

One of the most successful applications of HTCM is the study of peritectic reactions in Fe–C and Fe–Ni alloys, and proficient mastery of this equipment can play an essential role in the study of high N alloys. Li et al. [10] used HTCM to study the solidification mode of 316H austenitic stainless steel under rapid cooling, determined it to be a ferrite-austenite mode, and claimed that the δ-ferrite transformed into austenite through peritectic reaction. However, the typical peritectic reaction was not observed in its HTCM results.

HTCM can achieve sharp images due to its unique shallow depth of focus, but unfortunately, this feature is also one of the Achilles’ heel of this device. In essence, HTCM is also a simulation experiment, taking tiny samples from large ingots and simulating the solidification behavior of the entire billet under given conditions. Due to the small size of the sample, compared to the ingot, when the sample melts, the surface tension of the melt combines with the shallow depth of focus leading to the formation of a pronounced meniscus. Figure 1(a) illustrates the restricted field of view of the conventional HTCM, where the meniscus in the liquid phase results in the formation of localized highlight region. This makes it difficult to fully capture the liquid/solid interface across the entire field of view, resulting in poor imaging of interface progression.

Figure 1 (a) HTCM results during the controlled cooling of a hypo-peritectic sample. (b) Schematic representation of the HTCM chamber and concentric solidification technique, showing the liquid pool and solid rim in a SASS sample, redrawn from Reid et al. [11].
Figure 1

(a) HTCM results during the controlled cooling of a hypo-peritectic sample. (b) Schematic representation of the HTCM chamber and concentric solidification technique, showing the liquid pool and solid rim in a SASS sample, redrawn from Reid et al. [11].

In the present research, the invention of the concentric solidification method solved the observation blemish of conventional HTCM. Utilizing this original method to study high nitrogen stainless steel, a typical peritectic solidification was perfectly observed.

2 Materials and methods

The chemical composition of the S31254 SASS is shown in Table 1, which contains 0.2 wt% nitrogen. The alloying element N will play a crucial role in the subsequent solidification behavior research. For concentric solidification experiments, the sample dimensions are 10 mm in diameter and 0.25 mm in thickness.

Table 1

Chemical compositions of samples (wt%)

Fe Cr Ni Mo Mn Cu Si N C
S31254 Bal. 21.4 18.1 6.9 0.65 0.7 0.48 0.2 0.01

In order to solve the above-mentioned problem, the High Temperature Microscopy Laboratory at the University of Wollongong, began to develop the concentric solidification technique on the old 1LM21 equipment around the year 2003. In 2004, Reid et al. [11] demonstrated the application of concentric solidification to peritectic reaction in low carbon steel for the first time. The surface tension balance between solids, liquids, gases, and the crucible results in minimizing the formation of menisci on the liquid pool, greatly improving the quality of in-situ observations. Later, through this technique, Phelan et al. [12] proposed a new mechanism of peritectic reaction controlled by the dissipation rate of latent heat released by phase transformation, rather than the commonly believed control mechanism of solute diffusion in the liquid phase. Niknafs et al. [13] used this technique to study the interfacial instability during non-equilibrium solidification process of low carbon steel.

Concentric solidification technique refers to the formation of a centralized melt pool surrounded by a solid rim under radial thermal gradient. In the present research, a sample with a size of 10 mm in diameter and a thickness of 0.25 mm was fixed at the upper focus point of an infrared heating furnace with a gold-coated oval chamber through a platinum holder, and the halogen lamp heating source was located at the lower focus point of the chamber, as depicted schematically in Figure 1(b).

Normally, the temperature needs to be calibrated before starting the HTCM experiment. However, since the size of the sample used in the concentric solidification experiment is much larger than that of the ordinary HTCM sample, the temperature gradient is also steeper. The marginal temperature cannot represent the actual temperature when the reaction occurs. Although this study focuses on the peritectic reaction, for the actual temperature, Dr Dasith [14] gave a feasible method to calculate the temperature gradient of the samples.

3 Results

Concentric solidification is a new HTCM method which was first created to study the peritectic reactions [15,16]. For S31254 SASS at room temperature, it contains almost 100% γ and small number of secondary phases, mostly sigma phase (σ), as shown in Figure 2(a). When it was heated, the σ phase became darker and more explicit, which is a phenomenon called thermal etching, then the γ transformed into δ and started melting partially (Figure 2(b) and (c)).

Figure 2 HTCM snapshots revealing melting and solidification process of S31254 SASS under a cooling rate of 20°C·min−1 with temperatures of (a) 138°C；(b) 945°C; (c) 1302°C；(d) 1330°C; (e) 1322°C; and (f) 1254°C.
Figure 2

HTCM snapshots revealing melting and solidification process of S31254 SASS under a cooling rate of 20°C·min−1 with temperatures of (a) 138°C；(b) 945°C; (c) 1302°C；(d) 1330°C; (e) 1322°C; and (f) 1254°C.

The temperature is controlled manually instead of sticking to preset program. By carefully manipulating the temperature panel, a liquid pool was formed surrounded by δ. During the solidification process of S31254 SASS, the melt first takes δ-ferrite as the nucleation phase, i.e., the primary phase, to grow. As the temperature decreases, the solidification continues, and γ nucleates grows at the interface between δ-ferrite and liquid, and grows in both directions of liquid and δ-ferrite. The solid-state growth of γ proceeds at a much higher rate than liquid-state growth (Figure 2(d–f)).

4 Discussion

Early theories of the peritectic reaction were established based on the equilibrium phase diagrams [17], including Fe–C and Fe–Ni alloy phase diagrams. Simplifying SASS to Fe–Ni alloy, the peritectic range is 4–5 at. pct (3.7–5.1 wt%) Ni. Peritectic solidification consists of two steps. The first step is the peritectic reaction, γ grows along the L/δ interface (L + δ → γ) [16]. The second step is subsequent peritectic transformation, the pre-formed γ through peritectic reaction grows into δ and L phase [18,19]. Kerr et al. split this transition into three distinct regimes: reaction, transformation, and solidification [20].

No matter how the peritectic reaction was classified, it was crystal clear that the phenomenon observed by concentric solidification (Figure 3(a)) method is a typical peritectic reaction. The peritectic solidification was deeply explained in Fe–C steel which could also be used to describe the high N alloys. Arai et al. [4] studied the peritectic reaction of Fe-4.86 at. pct Ni with the HTCM technique and the results are shown in Figure 3(b). Austenite appeared at the triple point of L and δ, it grew rapidly along the L/δ interface and then thickened slowly into L and δ. With further cooling, a preferred growth of γ along the δ grain boundaries was observed. The γ extended perpendicularly from the lateral γ/δ interface.

Figure 3 HTCM revealing (a) the tri-phase coexistence of S31254 SASS and (b) the peritectic reaction of Fe-4.86 at. pct alloy [4].
Figure 3

HTCM revealing (a) the tri-phase coexistence of S31254 SASS and (b) the peritectic reaction of Fe-4.86 at. pct alloy [4].

In previous studies [21,22], the author used another in-house built experimental method, high temperature confocal microscopy – differential thermal analysis, to summarize and classify the solidification modes of SASS and duplex stainless steel, and analyzed them based on diversification of N content. A competitive nucleation mechanism in high-nitrogen stainless steel was also proposed. These studies focused on the nucleation of primary phases and subsequent phase transformations. In solidification processes involving multi-phase, how the phases involved transition between each other has not been effectively summarized. In this experiment, the peritectic reaction observed by the concentric solidification method complemented the solidification mechanism of high-nitrogen stainless steel. However, previous studies have shown that the solidification pattern of high-nitrogen stainless steel is greatly affected by the nitrogen content. Therefore, subsequent research on the role of nitrogen in peritectic reactions was still required.

5 Conclusions

The concentric solidification method was proved to be a practical tool for studying the multi-phase-involved solidification process. For S31254 super-austenitic stainless steel, γ transformed to σ at elevated temperature, and a δ-ferrite/liquid interface was created manually with care. During the solidification process, δ grew into the melt and then, γ started forming at δ-ferrite/liquid interface through peritectic reaction, which is L + δ → γ. The newly formed γ grew toward both solid and liquid by consuming δ and liquid. The capture of peritectic reaction improved the solidification mechanism of high nitrogen stainless steel.

Acknowledgements

The authors would like to thank Dr Suk-Chun Moon from UOW high temperature microscopy lab, and the authors’ PhD supervisors, Prof. Huijun Li, Dr David Wexler, and Dr Dominic Phelan.

  1. Funding information: Natural Science Foundation of Jiangsu Province (BK20201467), Scientific Research Funding Project of “333 High-level Talents Training Project” of Jiangsu Province (BRA2020260), Jiangsu Province “Six Talent Peaks” High-level Talent Selection and Training Funding Project (JZQC-03), and National Nature Science Foundation of China (NSFC)Grant No. 51971100.

  2. Author contributions: Tong Wang: writing – original draft, writing – review & editing, methodology, formal analysis; Sicheng Qian: visualization; Yu Wang: writing – review & editing; Yunfei Ding: project administration; Yiqiang He: project administration; Jilin Xu: methodology; Hao Xue: data analysis; Wen Feng: formal analysis; Feng Shang: formal analysis.

  3. Conflict of interest: Authors state no conflict of interest.

  4. Data availability statement: Original data could be reached through e-mail contact with corresponding author.

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Received: 2024-05-08
Revised: 2024-06-09
Accepted: 2024-06-12
Published Online: 2024-12-24

© 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-2024-0044
Keywords for this article
high nitrogen stainless steel; in-situ observation; concentric solidification; peritectic solidification
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  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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