1. Introduction
P91 steel belongs to a family of 9–12% Cr ferritic creep resisting steels [
1]. The steel was initially developed in the 1970s for application in steam generators of fast breeder reactors by Oak Ridge National Laboratory [
2], [
3]. At present P91 steel has wide application in high-temperature and high pressure components such as headers, heat exchangers, water-wall tubing and piping systems of fossil-fuel power plants[
4], [
5]. The suitability of this steel for these applications is due to its superior thermal mechanical properties. These include high corrosion resistance, good weldability and low thermal expansion [
6]. The steel also has toughness and good creep performance at temperatures up to 600 °C and 100,000 hours. This is due to carbides that evolve during tempering heat treatment during production [
7], [
8].
After prolonged service, the steel experiences internal damage due to microstructural changes from long-term exposure to high temperatures under stress. These microstructure changes cause a detrimental effect on mechanical properties, especially toughness and degradation of creep properties [
9,
8]. At the end of the design lifetime, the creep-exhausted components are replaced. The high cost of replacing these components has attracted research interest in extending the service life of creep-exhausted components.
Restoration of the microstructure of degraded components has been achieved through various thermal procedures such as heat treatment and hot isostatic pressing [
10]. Thermal rejuvenation procedures can modify the material's microstructure, thus improving mechanical properties[
11]. Heat treatment schedules may cause grain refinement and re-establishment of the original microstructure. The heat treatment can therefore restore the material properties of service-exhausted components [
12]. However, there is scanty information about the effect of rejuvenation heat treatment on metal flow behaviour, especially P91 steel.
In 9–12% Cr ferrite steels, heat treatment is generally by normalising, cooling and tempering processes [
13]. Normalising is conducted above the upper critical temperature, Ac
3, and tempering below the lower critical temperature, Ac
1 [
14]. Various authors [
2], [
8], [
14]–[
17] have applied different normalisation and tempering temperatures for P91 steel within the Ac
3 and Ac
1 requirements. Pandey
et. al. [
2] reported phase transformation temperatures of P91 as 810℃ to 825°C (Ac
1) and 912℃ to 930°C (Ac
3). According to Abe [
18], the Ac
1 was (800 to 830°C) and Ac
3 (890 to 940°C) in P91. The variations in heat treatment temperatures of P91 are due to minor differences in chemical composition (especially Ni + Mn), rate of heating and prior austenite grain boundaries(PAGBs) [
17]. American Society of Mechanical Engineers (ASME) [
18] recommended austenitisation temperature of 1040 to 1080°C and tempering at 730 to 780°C in P91 pipes.
In 9-12%Cr ferritic steels, creep deformation mechanisms are mainly associated with changes in the microstructure. These microstructure changes cause a reduction in dislocation density, migration of sub-grain boundaries, formation of new secondary phases (Laves and Z-phase) and growth of sub-grain structure [
19]. During creep, the sub-grains grow, causing a decrease in the creep strength in 9-12%Cr steels while Laves phase coarsens around M
23C
6 carbides along the PAGBs reducing their pinning effect [
20]. Hence, reducing the strengthening mechanism.
Heat treatment of P91 steel produces a tempered lath martensite structure with carbides such as M
23C
6 (M = Chromium, Iron, Tungsten and Molybdenum) and MX (M =Niobium, Vanadium and X-carbon) [
2]. During normalisation, the homogenisation of the microstructure occurs, causing an untampered lath microstructure with a small number of precipitates and a high dislocation density. Tempering causes the precipitation of the M
23C
6 carbides along the grain boundaries and MX particles in the matrix [
20]. The high dislocation density and M
23C
6 precipitates are responsible for the pinning of lath boundaries, while MX precipitates prevent dislocation movement [
2], [
21]. The heat treatment process, therefore, restores the effects of the creep deformation process and provides a stable microstructure that enables P91 steel to achieve high creep strength [
6].
Rejuvenation heat treatment, as mentioned earlier, can be used for complete recovery of material properties and reuse of exhaust components or partial recovery for alternative applications [
10]. Should the alternative application require the manufacturing of a new structural part from either processing or machining, it is imperative to understand the response of the effect of rejuvenation heat treatment on creep-exhausted steel to thermomechanical processing parameters. Hence, the study provides the basis for understanding the metal flow pattern during deformation. A comparative study using constitutive models developed from the hot deformation behaviour of steel A and steel B can be used for this analysis [
22].
For example, phenomenological constitutive models such as Arrhenius equations are widely used to study the metal flow behaviour of various metals and alloys [
23]. Examples of such materials include low-carbon steel [
24,
25], P92 steel [
26], nickel-based super alloys [
27], alloys of aluminium [
24], and magnesium [
28]. The accuracy and reliability of a constitutive model in predicting the flow stress form the basis of studying the material process behaviour [
29]. These models act as inputs to Finite Element Method codes. These computer codes assist in the simulation and the optimisation of thermomechanical process parameters. The simulation results depend on the accuracy and dependability of the constitutive models [
22], [
29].
The objective of the present study was to investigate the flow stress behaviour of steel A and steel B using constitutive equations. The steel B was heat treated by normalisation followed by air cooling, then tempering processes. Isothermal hot deformation tests were then conducted at various strain rates and temperatures to study the flow stress behaviour for the two steels. Experimental flow stress values were used to develop constitutive equations based on the Arrhenius-type equation. These equations were validated using statistical parameters.
2. Materials and Methods
The P91 steels studied had chemical composition (wt%) of Cr-9.189 C-0.1 Mn-0.447 Mo–0.885 V–0.191 Nb-0.076 Ni–0.158 Si-0.254 P-0.02 Cu-0.086. Isothermal compression samples were machined from the two steels to a cylindrical shape of diameter 8mm and height 12 mm. The steel B samples were heat treated by austenitising at 1050°C for 40 minutes, air cooling and tempering at 760°C for 2 hrs, as shown in
Figure 1. These are typical heat treatment conditions used during the production process of boiler pipes [
16]. Figure 3 (a) and (b) show the optical micrographs of undeformed steel A and steel B. The steel A showed a typical tempered martensitic microstructure with prior austenite grain boundaries (PAGBs) and dispersion of fine precipitates in the matrix. The microstructure of steel B exhibited clear grain boundaries compared to steel A.
The uniaxial hot compression parameters using Gleeble® 3500 equipment were as follows: deformation temperatures of 900°C, 950°C, 1000°C, and 1050°C and strain rates of 0.01s
−1, 0.1s
−1, 1s
−1, and 10s
−1 to a strain of 0.6. Before testing, an R-type thermocouple was welded at the midpoint on the samples to monitor temperature during the deformation process.
Figure 2 is a schematic diagram illustrating the thermal deformation process used in this study. All the specimens were heated at 5°C/s to 1100°C and held isothermally for 180s before cooling to the deformation temperature.
The deformed samples were cut along the compression axis for microstructural analysis. The specimen was prepared following the metallographic procedures. Etching was done using Villella’s reagent solution (1g Picric acid + 5 ml HCl + 100 ml ethanol).
Figure 3.
The optical micrographs for a) steel A b) steel B.
Figure 3.
The optical micrographs for a) steel A b) steel B.
4. Conclusion
In this study, the hot deformation behaviour of P91 steel was studied using a Gleeble® 3500 thermo-simulation machine on steel A and steel B. The deformation conditions were: a temperature range of 900°C to 1050°C and strain rates of 0.01 to 10s−1. The findings are as itemised below:
The flow stress-strain curves show that the flow stress increased with an increase in strain rate (0.01 s−1 to 10s−1) and decreased with an increase in temperature (900°C to 1050°C) for the two steels. The flow stress-strain curves exhibited a DRV+WH as the deformation mechanism.
The apparent activation energy of steel A was 473.08 kJ/mol, and for steel B was 564.48 kJ/mol. These Q-values were much higher compared to self-diffusion energy of iron in austenite (270 kJmol−1)
The mathematical constitutive models for steel A and steel B to strain of 0.6 are as given in Equation (22) and (23).
The constitutive models for steel A and steel B were used to predict flow stresses. The models were then validated using Pearson’s correlation coefficient, R and Average Absolute Relative Error, AARE. For steel A, R was 0.97, and AARE was 7.62%. For heat-treated creep-exhausted P91 steel, R was 0.98, and AARE was 6.54%. These results show a good correlation between experimental and predicted values. The developed models for the two steels can be used interchangeably with acceptable accuracy. Using the model for steel A on steel B, Pearson’s correlation coefficient was 0.96, and AARE was 7.19%. Similarly, using the steel B model on steel A, the R-value was 0.95, and AARE was 8.36%.