Work hardening and X-ray diffraction studies on ASS 304 at high temperatures

A. Anitha Lakshmi; Alok Bhadauria; Ashish Kumar; Rakesh Chandrashekar

doi:10.1515/htmp-2024-0008

Article Open Access

Work hardening and X-ray diffraction studies on ASS 304 at high temperatures

A. Anitha Lakshmi , Alok Bhadauria , Ashish Kumar and Rakesh Chandrashekar

Published/Copyright: May 10, 2024

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From the journal High Temperature Materials and Processes Volume 43 Issue 1

Abstract

One of the most common characteristics of metallic alloys is work hardening, which is most beneficial as it is the primary reason for the alloys’ tenacity to withstand loading even in the presence of internal flaws or geometrical errors. Thus, the work hardening coefficient gives the maximum amount of homogeneous plastic deformation in tensile straining. Thus, complex-forming operations are facilitated by a high coefficient without experiencing premature failure. Naturally, work hardening has a significant impact on the mechanical energy required to shape a material by plastic deformation, such as rolling, forming, etc. The quantity of energy that the material stores during plastic deformation is also managed by work hardening. As a result, it significantly influences how the metal behaves when it is subsequently softened during annealing. Finally, the hardening capacity and durability of the work hardened state are significant practical challenges because many high-volume stretch formed components are directly used. Typically, the current study begins, at homologous temperatures above 0.4 times melting point, with a description of work hardening at 700, 800, and 900°C temperatures in three different orientations with respect to rolling direction R ₀, R ₄₅, and R ₉₀ and 10⁻¹−10⁻³ s⁻¹ strain rates, where thermally triggered processes exhibit a prominent role in work hardening. Three stages of behavior were identified by analyzing the tensile work hardening of ASS 304 steel. Dynamic strain aging is the cause of the anomalous fluctuation in the work hardening rate that is seen in hot working temperatures. X-ray diffraction examination is conducted to introspect any phase changes occurring in hot working regions improving plasticity of ASS 304.

Keywords: work hardening; hot working; XRD; EDAX; plasticity deformation

1 Introduction

The strengthening of a material via extremely low-temperature plastic deformation is referred to as work hardening or strain hardening [1,2,3]. One of the most prevalent features of metallic alloys is work hardening, which is also likely the most beneficial because it is the primary reason for their tenacity – that is, their ability to withstand loading even in the presence of internal defects or geometrical defects [4,5,6,7]. The work hardening coefficient specifies the greatest percentage of homogeneous deformation caused by plasticity in tensile straining. Thermally activated processes greatly influence plastic deformation at hot forming temperatures above 0.4 T _m, making temperature, strain, and change in strain with time dependent [8,9,10,11,12]. Climbing and cross-slip mechanisms continuously destroy the dislocations during deformation, which causes the dislocation substructure to significantly recover dynamically. These processes are primarily governed by local atomic diffusion. As a function of temperature, this significantly lowers the flow stresses, which eventually tend to saturate at values [13,14,15].

A thorough examination of work hardening in sheet material can help to maximize the process of hot forming of pure metals and alloys [16]. Numerous studies with respect to work-hardening characteristics of various materials have been carried out in the past [16,17]. For a C–Mn steel, the rate of work-hardening because of yielding and saturated stresses, in addition to thermodynamic assisted rate of work-hardening and the flow stress, were determined employing differentiation representation of empirical equation [18].

2 Materials and methods

Hot tensile tests are carried out for investigating the work-hardening attributes of ASS 304 at elevated working temperatures. The tests performed include a wide range of deformation temperatures, from 700 to 900°C, at three distinct strain rates. Consequence behaviors like strain rate, temperature related deformation, and strain upon work hardening are examined based upon experimental data. Plotting the rate of fluctuation strain hardening, θ (=dσ/dε), against plastic strain on a log-log scale allows one to visualize the work hardening tendency. For the investigation of work hardening behavior, the original Crussard and Jaoul [19] plots are used in terms of θ (=dσ/dε) against ε. Subsequently, They [20] noted that, depending on past deformation history, different work hardening regimes depicted by such plots were prone to variations.

They proposed that it would be more appropriate to analyze plots in terms of θ against σ because different regimes of these plots are independent of the previous deformation history [21,22,23]. These figures show that the alloy exhibits two regimes under all circumstances: regime I, which shows a rapid decrease in strain hardening rate, and regime II, which shows a constant strain hardening rate [24,25,26,27,28,29,30,31,32]. This work has looked at log-log scale plots of θ vs ε (Figure 1a) and θ vs σ (Figure 1b). It is discovered that they are rather comparable in that both types of plots display two separate strain hardening regimes, and the rates of strain hardening for the various regimes are nearly the same in both cases. They show no deviations from what the previous investigators reported. This behavior is most likely caused by the alloy’s casting state, which prevented it from having undergone any previous deformation, throughout the current investigation. Furthermore, when plotted in terms of θ vs σ as opposed to θ vs ε plots, the curves for various heat treatment conditions are clearly separated, at least in regime I, as shown in Figure1b.

Figure 1

The strain hardening rate, θ (=dσ/dε), varies according to two factors: (a) strain and (b) stress in the particular case of Ass 304 at hot forming temperatures of 0.01 s⁻¹.

The rate of strain and deformation temperature have an impact on the work-hardening rate. The rate of work-hardening usually decreases with respect to the increase in deformation temperature, drop in strain with respect to time at a fixed strain (less than 0.3). Under the conditions of lower strain with respect to time and high deformation temperature, dislocation density noticeably will be modest.

The most widely used X-ray-based analytical technique for material characterization is likely the process of X-ray diffraction (XRD) analysis. As the name implies, the sample is typically in the form of a finely ground crystalline substance that has to be investigated. In actuality, the word “powder” refers to the sample’s crystalline domains being orientated randomly. As a result, the different d spacings in the crystal lattice are represented as concentric rings of scattered peaks in the 2D diffraction pattern that is recorded. The fundamental structure (or stage) of a material can be determined by looking at the locations and intensities of the peaks. For instance, despite the fact that both graphite and diamond are composed of carbon atoms, their diffraction lines would differ. Because structure has a significant influence on material properties, phase identification is crucial [33].

Regular, repeating atomic planes that make up a crystal lattice establish the theory as well as the method of the three-dimensional arrangement of crystalline substances such as minerals. A concentrated X-ray beam reacts with these atomic planes in a way that causes some of the beams to be transmitted, some to be absorbed into the sample, some to be diffracted, scattered, and refracted. Depending on which atom constitutes the crystal’s lattice and how they are organized, each mineral diffracts X-rays differently. When an X-ray beam meets a sample and is diffracted, it can be used to measure the distances that separate the plane within the atoms that make up the sample [34]. Bragg’s Law was first presented in 1921 and is named after William Lawrence Bragg. Bragg’s Law is given as

(1) n λ = 2 d sin θ ,

where λ is the incident X-ray beam’s wavelength, d is the separation between consecutive atomic planes (the d-spacings), n is the diffracted beam’s integer order, and θ is the X-ray beam’s angle of incidence.

Equation (1) is utilized to calculate d-spacings based on the supplied variables. An XRD’s geometry is made to allow for measurement. The distinctive set of d-spacings generated in a typical X-ray scan provides the unique “fingerprint” of the substance or elements in the sample. This “fingerprint” aids in material identification when properly interpreted and compared to standard reference patterns and proportions. XRD analysis is a widely used technique in material science. It can be used to measure crystallite size, particularly in nanomaterials, identify phase transitions in an experiment, semi-quantitatively determine what phases are present in a sample, analyze stress in a sample, and examine crystal structure [35,36,37].

XRD studies are performed on the ASS 304 stainless steel fractured specimens at room temperature (RT), 700, 800, and 900°C temperatures. At 900°C temperature, XRD on specimens is performed in rolling direction R ₀, diagonal direction R ₄₅, and transverse direction R ₉₀ to investigate the difference in XRD patterns.

In hot working temperature range, XRD on fractured specimens is performed in rolling direction R ₀ in the temperature interval of 100°C. The outcome validates that at RT, these materials display FCC systems and hexagonal close-packed systems, respectively. To examine the various phases generated along the line of contact due to diffusion at different heating temperatures, XRD is performed on the fracture side of the samples. Figure 2 Represents XRD analyses of fractured surfaces for specimens at 900°C in Ro, R45, and R90 orientation, respectively.

$Figure 2 XRD analyses of fractured surfaces for specimens at 900°C in R o, R 45, and R 90 orientation, respectively.$

Figure 2

XRD analyses of fractured surfaces for specimens at 900°C in R _o, R ₄₅, and R ₉₀ orientation, respectively.

3 Results and discussion

3.1 Work hardening phenomena in Ass 304 at hot working temperatures

At lower temperatures and elevated strain rates, it is noticed that splits become twisted and stored inside the grains. The low deform temperature is the reason for the slow vacancy diffusion rates. The pace at which discontinuities are produced increases in tandem with the strain rate. In a weak stacking fault energy alloy, the dislocation rises and cross-slips when it encounters an obstruction (i.e., vacancy, a dislocation, grain boundary). Dynamic recuperation takes place gradually. The complex and crossing high-density dislocations that give rise to the network architecture make the dislocation slip difficult. The flow stress greatly increases when temperature increases because of the dislocation strengthening (Figure 3).

Figure 3

Work-hardening rate variations with actual stress for the ASS 304 at excessive temperatures of operation in the R _o orientation.

Several variables, including severe oxidation, grain development, or an undesired phase shift, influence the maximum temperature for hot working. To minimize forming forces and extend the time available for hot working the workpiece, materials are typically heated to their maximum point first in practice.

Dynamically recrystallized grains and some sub grains emerge at 900°C (high temperatures and moderate strain rates). It is known that the movement of dislocation is a thermally triggered process. At an extreme deformation temperature, sufficient energy can be created to facilitate dislocation movements such as climb, dislocation slip, and cross-slip. Once built up near grain boundaries, the gaps are recombined to produce sub-grain borders and dislocation cells. The protracted deformation period provided by the low strain rate allows the grain boundary to diffuse and migrate, and eventually the dynamically recrystallized grain will gradually become visible. As the temperature of deformation rises, there is a greater dislocation movement, which encourages the process of dynamic recrystallization. This leads to increased plastic deformation as strain increases (Figure 4). When the strain rate is lowered to 0.0001 s⁻¹ and the change in temperature is increased to 900°C, the dynamic recrystallization proceeds quickly. As a result, there is confusion regarding the relationship between the work-hardening rate, actual stress, and the DRX incubation stage. The vital strain point (ε _o) of a material is the smallest amount of the true strain at which the first break emerges. Once the strain exceeds the critical strain, dynamic recrystallization takes place. The ever-present softening tendency is so visible at this moment. More straining results in a progressive decline in the rate of work-hardening to zero as the rate of stress reaches the peak stress. The energy needed for dislocation movements such as dislocation slip, climb, and cross-slip can be obtained from high deformation temperatures. In the area around grain boundaries, the dislocations are stacked up and then recombined to form sub-grain borders and dislocation cells. The microstructural investigations at various deformation phases at 900°C, 10⁻³ s⁻¹ demonstrated a complicated evolution, i.e., increased strain activated various deformation mechanisms. First, a reorganization of the dislocations causes impurities to develop, which are then triggered by locking the deformation that was first caused by an increase in load. After that, resistance was noticed due to locking of the deformed sites. Eventually, an accumulation of stress at the dislocation site triggers a constant dynamic recrystallization.

Figure 4

Shows how the ASS 304’s work-hardening rate varies with real strain at all strain rates and temperatures.

3.2 XRD spectrometer

The XRD (Figure 5) of fractured specimens at 700, 800, 900°C, and RT signify that compared to RT the intensity of peak is reduced for specimen at 800°C. The number of smaller peaks at RT disappears in the specimens at a higher temperature. The difference in the intensity of peaks at hot working temperatures indicates the formation of intermediate phases. These phases can be witnessed in the SEM micrographs where precipitates and carbides of chromium (Figure 6) are observed. The energy-dispersive X-ray spectroscopy (EDS) % weight composition of elements present at hot working temperatures too evidenced the presence of chromium in the fractured samples which substantiate the formation of new phases which in turn influences the enhancement of ductility at hot working temperatures. The creation and spread of vacancies in metallic materials are favorably influenced by higher temperatures. During the dislocation climb, vacancies may directly attach to the jogs or may jump into the dislocation core and then diffuse to the jogs on the dislocation. Dislocation climb is a non-conservative motion since it necessitates the absorption or emission of vacancies and moves the dislocation on a plane perpendicular to its slip plane. The improved vacancy diffusion causes the climb rate to rise with temperature. Because of this, dislocation pile-ups at other obstacles can be relieved by climbing, which increases the flexibility of materials by allowing dislocations to continue gliding on other slip planes. Thus, at elevated temperatures, vacancy diffusion-induced dislocation climb represents a significant inelastic deformation mechanism.

$Figure 5 XRD analyses of fractured surfaces at RT, 700, 800, and 900°C in R 0 orientation.$

Figure 5

XRD analyses of fractured surfaces at RT, 700, 800, and 900°C in R ₀ orientation.

Figure 6

SEM micrographs showing the broken surface of ASS 304, 1 mm thick, in R ₉₀ orientation, magnified 10,000 times. (a) 700°C, (b) 750°C, (c) 800°C, (d) 850°C, and (e) 900°C.

The XRD patterns indicate that certain structural alterations occur after heating. The diffractogram shows these changes as the emergence of new peaks. It is also evident that the peaks’ strength rises with temperature. All peaks vanish when the composition melts at some point. The peaks indicate the crystallinity of the material. From Figure 5 it can be seen that a high intensity peak compared to RT indicates a high level of crystallinity in the phase resulting in the formation of chromium carbides locking the deformation thereby increasing the resistance to load applied. A similar tendency can be seen at 700 and 800°C. If we observe the peaks in Figure 5, the width of the peak is more at 800°C indicating more strain hardening. EDS results shown in In Figure 6 and composition values from Table 1 indicate the formation of new compounds or inclusions like chromium carbide resulting in dynamic strain aging.

Table 1

ASS 304 steel percentage composition in the EDS report at 0.001 s^–1 rolling direction R ₀ and 1 mm thickness at (a) 700°C, (b) 750°C, (c) 800°C, (d) 850°C, and (e) 900°C

Temperature	700°C	750°C	800°C	850°C	900°C
Element	Weight percentage
C	12.02	25.57	12.19	11.46	22.09
O	4.68	17.7	21.94	24.17	25.66
Si	0.96	0.73	0.57	0.75	1.38
Cr	15.97	12.01	15.64	14.31	8.21
Mn	0.80	0.65	1.79	1.68	0.96
Fe	56.79	36.11	45.02	43.10	35.97
Co		0.32	0.39	0.25
Ni	5.43	3.31	2.41	2.8	1.71
Mo		0.52	0.06	0.05	0.46
Na	1.13	1.49		0.88	0.94
Cl	0.76	0.99		0.55	1.08

In Figure 6 SEM micro-graphs showing the voids, carbide precipitates and dimples at 700°C, 750°C, 800°C, 850°C, and 900°C represent phase formation evidenced in Table 1. EDS shows the kinds of chemical elements that are present in surface fractures. Some of the chemical components found in the broken surface are traced in the EDS report. The elements, including Cr, Co, Mn, Ni, Mo, and Si, are confirmed by these reports.

The fractured surface contains inclusion, based on the EDS data shown in Figure 7. Carbon and chromium make up most of the inclusion. Table 1 suggests that the complex carbide in question may be mostly composed of carbon and chromium, as seen by the lower percentage of elongation in the R ₄₅ and R ₉₀ directions when compared to the R ₀ direction.

Figure 7

EDS report for ASS 304 steel shattered surfaces at various temperatures with a 1 mm thickness at 0.001 s⁻¹ in the rolling direction R ₀. (a) 700°C, (b) 750°C, (c) 800°C, (d) 850°C, and (e) 900°C.

4 Conclusion

This research focused on studying the work hardening behavior and XRD analysis of ASS 304 at hot working temperatures. Work hardening graphs are developed and XRD analysis is carried for ASS 304 at 700 and 900°C by experimentation, these investigations bring out the following outcomes:

The grain boundary can diffuse and migrate over a lengthy period due to the low strain rate. This allows the grain to progressively recrystallize dynamically. Elevated deformation temperature at 800°C and 10⁻³ s⁻¹ strain rate causes an increase in dislocation mobility, which in turn encourages dynamic recrystallization and subsequently leads to increased plastic deformation and strain.
The EDS report, demonstrating traces of chemical components available in the cracked surface, supports XRD report’s finding of the presence of a new phase with high intensity peak. Most of the inclusion is made up of carbon and chromium which might be a complicated carbide with a higher percentage of elongation.
The ductility of the material increases with the increase in forming temperature and strain rate but at 900°C, the strength of the material is reduced twice compared to 800°C. Thus, there is enhanced formability up to 850°C balancing with the strength of the material.

Acknowledgments

The authors express their gratitude to GRIET, Hyderabad and MIT, MAHE Bengaluru Campus for their supply of facilities and financial assistance. The authors acknowledge their gratitude for the valuable input and ideas provided by the anonymous reviewers, guest editor, and editor-in-chief, which greatly enhanced the quality of the work.

Funding information: The authors state no funding involved.
Author contributions: Conceptualization: A. Anitha Lakshmi, Ashish Kumar, and Rakesh Chandrashekar; methodology: A. Anitha Lakshmi, Ashish Kumar, and Rakesh Chandrashekar; investigation: Rakesh Chandrashekar; data curation: A. Anitha Lakshmi, Ashish Kumar, and Rakesh Chandrashekar; formal analysis: Alok Bhadauria, Ashish Kumar, and Rakesh Chandrashekar; resources: A. Anitha Lakshmi, Alok Bhadauria, Ashish Kumar, and Rakesh Chandrashekar; supervision: A. Anitha Lakshmi and Rakesh Chandrashekar; validation: A. Anitha Lakshmi, Ashish Kumar, and Rakesh Chandrashekar; writing – original draft: Ashish Kumar and Rakesh Chandrashekar; writing – review and editing: A. Anitha Lakshmi and Alok Bhadauria.
Conflict of interest: The authors state no conflict of interest.
Author statement: This article has been written by the stated authors who are all aware of its content and approve its submission. This article has not been submitted anywhere else for parallel publication.
Ethical approval: The conducted research is not related to either human or animal use.
Data availability statement: All data generated or analyzed during this study are included in this published article.

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Received: 2024-02-18

Revised: 2024-03-18

Accepted: 2024-03-20

Published Online: 2024-05-10

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

Articles in the same Issue

https://doi.org/10.1515/htmp-2024-0008

Keywords for this article

work hardening; hot working; XRD; EDAX; plasticity deformation

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BY 4.0