Optimization of hot working parameters for thermo-mechanical processing of modified 9Cr–1Mo (P91) steel employing dynamic materials model

Intrinsic workability of modified 9Cr–1Mo steel has been studied in a wide range of temperatures (1123–1373 K) and strain rates (0.001–10 s^?1). Using the experimental data obtained from isothermal hot compression tests, processing map at 0.5 true strain has been developed employing dynamic material model (DMM) approach. The activation energy map has been developed to substantiate the results obtained from processing map and to finalize the optimum processing parameters. Microstructural studies have been carried out to validate the domains of the processing map. The material shows localized deformation bands in the temperature range of 1150–1373 K at strain rates above 1 s^?1 and exhibits abnormally elongated martensite laths at higher temperature (1373 K) and lower strain rates (0.001–0.01 s^?1). The optimum domain for the hot deformation is found to be in the temperature ranges of 1250–1350 K and strain rate ranges 0.015–0.3 s^?1 with a peak efficiency of 38%. In this domain, apparent activation energy is found to be 400 kJ/mol. The microstructure of the specimens deformed in this region exhibits defect free equiaxed grains.     

Effect of test temperature on fracture toughness of modified 9Cr–1Mo steel

Abstract

The quasi-static fracture behaviour (J–R curves) of modified 9Cr–1Mo (P91) steel was studied. The J–R curves were established at 298, 653, 823 and 893 K, and fracture toughness J_0·2 at 0·2 mm of crack extension was determined. The value of ～J_0·2 at 653 K was lower compared to that at 298 K followed by increases in J_0·2 values at 823 and 893 K. The decrease in J_0·2 at 653 K can be attributed to the influence of dynamic strain aging. At 893 K, a significantly higher (more than 200%) J_0·2 was observed, since plastic deformation of the net section, rather than crack growth, occurred in this condition.     

Effect of dynamic plastic deformation on microstructure and annealing behaviour of modified 9Cr−1Mo steel

The effect of dynamic plastic deformation on the microstructure of a modified 9Cr?1Mo steel has been investigated in comparison with the effect of quasi-static compression. It is found that the boundary spacing after dynamic plastic deformation is smaller and the hardness is higher than those after quasi-static compression. The microstructure after dynamic plastic deformation is however less stable than the microstructure after quasi-static compression. Annealing at 675 and 700°C leads to structural coarsening and recrystallisation in each sample, but with recrystallisation occurring faster in the sample annealed after dynamic plastic deformation. The lower thermal stability of the microstructure produced by dynamic plastic deformation is attributed to a higher driving force for recrystallisation in the dynamically deformed material.     

Serrated yielding in 9Cr–1Mo ferritic steel

Abstract

Tensile tests were performed on specimens in quenched and tempered and thermally aged conditions over a wide temperature range (300–873 K) to assess the occurrence of serrated flow, a manifestation of dynamic strain aging (DSA), in 9Cr–1Mo ferritic steel, with an emphasis on the influence of prior thermal aging on serrated yielding. The alloy exhibited jerky/serrated flow in the load–elongation curves at intermediate temperatures. Types A, B, and C serrations were observed, depending on the test temperature and applied strain rate. The apparent activation energy of 83 kJ mol^-1 measured for serrated flow suggests that diffusion of an interstitial solute such as carbon is responsible for dynamic strain aging in 9Cr–1Mo steel. Prior thermal aging at 793 K for 5000 h and at 873 K for 1000 and 5000 h resulted in a significant decrease in the height of serrations, i.e. the magnitude of the stress drop, as well as an increase in the critical strain for the onset of serrations. Both of these observations indicate reduced propensity to DSA as a result of increased precipitate sinks as well as a reduced carbon concentration in solid solution owing to an increased density of carbides in the thermally aged conditions. Reduced propensity to DSA resulted in a significant reduction in the strength values at intermediate temperatures.     

Microstructure and tensile properties of modified 9Cr–1Mo steel (grade 91)

Abstract

The influence of different soaking temperatures in the range 973–1623 K (below Ac ₁ to above Ac ₄) before oil quenching and tempering, on the microstructure, hardness, grain size, and tensile properties of modified 9Cr–1Mo steel has been studied. This was done in an effort to assess the tensile behaviour of the different microstructures likely to be encountered in the heat affected zone of a fusion welded joint of the steel. The steel developed predominantly martensitic structure after quenching. Soaking of steel in the intercritical temperature range (between Ac ₁ and Ac ₃) reduced the prior austenitic grain size and hardness. Soaking temperatures above Ac ₃ increased the grain size and hardness of the steel until the formation of δ ferrite at temperatures above Ac ₄. The δ ferrite formation at soaking temperatures above Ac ₄ reduced the grain size and hardness of the steel. The tensile strength of the steel exhibited a minimum for soaking in the intercritical temperature range where the ductility was highest. Strength increased and ductility decreased with further increases in soaking temperatures above Ac ₃. The formation of δ ferrite at soaking temperatures above Ac ₄ improved the ductility. The tensile properties have been correlated with the microstructures.     

Hydrogen and temper embrittlement in 9Cr–1Mo steel

Abstract

The synergism between hydrogen embrittlement and temper embrittlement has been investigated in a 9Cr–1Mo martensitic steel. Measurements of tensile ductility were used to monitor the development of embrittlement with increasing hydrogen content in material as tempered and aged for up to 5000 h at 500 or 550°C. A detailed examination was made of associated changes in fracture mechanism, precipitate microstructure, and interfacial and precipitate chemistry. A strong interaction between hydrogen and temper embrittlement was observed. Both types of embrittlement in isolation reduced tensile ductility by promoting a ductile interlath fracture mechanism: ‘chisel fracture’. Hydrogen and temper embrittlement acted synergistically to reduce ductility further by the promotion of brittle intergranular fracture and transgranular cleavage. The dominant factor controlling the interaction was the precipitation of a brittle intermetallic Laves phase containing phosphorus in solution. Phosphorus segregated to interfaces was considered to make an important, but secondary, contribution to the embrittlement observed.

MST/791     

Cyclic creep behaviour under tension–tension loading cycles with hold time of modified 9Cr–1Mo steel

Abstract

Cyclic creep behaviour of modified 9Cr–1Mo steel was investigated by a series of cyclic creep (CC) tests at 600°C, which were performed under controlled tension–tension loading cycles with the magnitude of stress ranges in a constant stress ratio (R?=?0·1). Hold time was applied for a 10 min hold at the maximum stress (σ_max) and minimum stress (σ_min). The CC properties were compared with the static creep (SC) using Norton’s power law, Larson–Miller plot, and Monkman–Grant relation, and the microstructure was examined. For the test conditions employed in the present investigation, retardation in the CC behaviour in terms of a lower creep rate and longer rupture time compared to those in the SC was obtained. The retardation was ascribed to the effects associated with anelastic recovery during the 10 min hold time at the minimum load of the cyclic loading. The creep rupture ductility decreased with a general decrease in stress, and there was no difference in the creep ductility between the CC and SC. The steel displayed a transgranular fracture characterised by the presence of dimples resulting from micro-void coalescence. Carbide precipitation was more coarsened with increasing in exposure time in the CC tests.     

Zone-wise investigation of creep behaviour 9Cr–1Mo steel weld joints

Distinct regions such as weld metal, heat-affected zone (HAZ) and base metal of P9 steel weld joints fabricated by various welding processes were investigated using impression creep testing. Smaller prior austenitic grain size, lower density of precipitates and dislocations resulted in faster recovery and higher creep rate of HAZ in comparison to the weld and base metal. Compared to base metal, shielded metal arc weld (SMAW) and activated tungsten inert gas (A-TIG) weld of the P9 steel weld joints exhibited better resistance to creep and displayed higher activation energy due to their coarser prior austenite grain size. A-TIG HAZ exhibited superior creep properties compared to the SMAW and TIG HAZ due to the presence of higher number density of precipitates.     

Development of microstructure during heat treatment of high carbon Cr–Mo steel

Abstract

Stainless steels containing enhanced chromium and carbon contents are particularly attractive for applications requiring improved wear and corrosion resistance. The as cast microstructure of such steels is composed mainly of ferritic matrix along with a network of interdendritic primary carbides. It has been shown that heat treatment of these steels results in microstructures that contain more than one type of carbide. A selective dissolution technique has been employed to isolate carbides from the matrix. Scanning electron microscope and X-ray diffraction studies of the as cast steels have shown that the primary carbides are essentially of M₇C₃ type, whereas in heat treated specimens both M₇C₃ (primary) and M₂₃C₆ (secondary) type carbides have been observed. The relative amounts of these carbides are found to be dependent on the heat treatment temperature. In addition, nucleation of austenite occurs above 950°C and at ～1250°C the matrix transforms entirely to austenite, which is retained completely on quenching to room temperature.     

Influence of precipitation and segregation on hydrogen embrittlement in aged 9Cr–1Mo steel

Abstract

A study is reported of temper embrittlement and hydrogen embrittlement in a series of model 9Cr–1Mo steel alloys in which the levels of silicon and phosphorus have been varied to separate the formation of the brittle intermetallic (Laves) phase from the segregation of phosphorus during aging. Phosphorus segregation was mildly detrimental to ductility properties, Laves phase formation was more detrimental, and their effects combined produced the most severe loss in ductility. Hydrogen effects were additive to those of aging. In unaged material without silicon enrichment, only M₂₃C₆ precipitates were detected, with little phosphorus segregation. With silicon enrichment, phosphorus segregation to lath and grain boundaries was enhanced. This enhancement increased the susceptibility of the materials to hydrogen embrittlement, promoting transgranular cleavage and chisel fracture. In aged material, the high phosphorus alloys showed some grain boundary segregation, but only limited interaction with hydrogen. In the high silicon alloys, the formation of Laves phase was most evident. This enhanced hydrogen embrittlement resulted in extensive chisel, transgranular cleavage, and some intergranular fracture. In the high silicon high phosphorus alloy, both Laves phase formation and phosphorus segregation were evident. This resulted in enhanced susceptibility to hydrogen embrittlement, producing intergranular fracture. Thus, silicon controls the susceptibility to hydrogen embrittlement in unaged alloy by promoting phosphorus segregation and in aged alloy by promoting Laves phase formation. In the aged alloy, segregation of phosphorus can enhance the effect of silicon.

MST/1785     

Cleavage fracture in 26Cr–1Mo ferritic stainless steel

Abstract

Cleavage fracture of a 26Cr–1Mo ferritic stainless steel has been studied using fatigue precracked specimens. The parameters determined were fracture toughness, cleavage fracture strength, and effective surface energy of ferrite. The results have been compared with earlier results on notched specimens.

MST/185     

Thermo-metallurgical and thermo-mechanical computations for laser welded joint in 9Cr–1Mo(V,Nb) ferritic/martensitic steel

Transient thermo-metallurgical and thermo-mechanical computations for laser welded joint, in 9 mm thick 9Cr–1Mo(V, Nb) ferritic/martensitic steel plate, in square-butt configuration, have been carried out by simulating the laser welding process on the 3-dimensional (3D) solid model using a finite element based welding and heat treatment simulation solution package – SYSWELD. The heat source has been modeled as a combination of a 3D Gaussian and a double ellipsoid profiles for realistic representation of fusion zone morphology. Phase and temperature-dependent physical and mechanical properties of this material were used in these computations. The results show very short residence time (<0.5 s) for the material in the heat affected zone (HAZ). The results clearly delineate the effects of different thermo-metallurgical processes like heating, softening, cooling and solid state phase transformation (SSPT) on temporal evolution of the stress-field resulting from laser welding. Longitudinal component of the residual stress is the most significant followed by the normal component and the transverse component is the least significant. Cross-weld residual stress profiles show a trough in the fusion zone and the heat affected zone (HAZ) with a peak in the parent metal region bordering the metallurgical HAZ. Also, the longitudinal and the normal components of the residual stress show nearly similar profile with different magnitudes. The computed residual stress profiles show reasonably good agreement with that measured by neutron diffraction. The results also show significant plastic deformation and strain-hardening of the austenitic phase-field prior to its transformation into martensite.     

Effect of W–Mo balance on long-term creep life of 9Cr steel

The effect of tungsten–molybdenum (W–Mo) balance on creep life has been investigated for five heats of martensitic 9Cr steel with 1.5 % Mo equivalent (= 1/2W + Mo) at 600, 650 and 700°C. The combination of W and Mo concentrations in the present steel is 3W–0Mo, 2.8W–0.1Mo, 2.4W–0.3Mo, 1.8W–0.6Mo and 0W–1.5Mo. The time to rupture t_r exhibits a monotonous increase with increasing the W–Mo balance parameter 1/2W/(1/2W + Mo), namely, with increasing W concentration and concomitantly with decreasing Mo. The increase in t_r with increasing 1/2W/(1/2W + Mo) becomes less significant at long times. The precipitation of Fe₂(W,Mo) Laves phase takes place preferentially at prior austenite grain boundaries during creep, which enhances the grain boundary (GB) precipitation hardening. The amount of Laves phase increases with increasing 1/2W/(1/2W + Mo). The coarsening of Laves phase takes place at long times during creep, which reduces the GB precipitation hardening.     

Characterisation of long term aging behaviour of 9Cr–1Mo ferritic steel using ultrasonic velocity

Abstract

The measurement of ultrasonic velocity of 9Cr-1Mo ferritic steel thermally aged at 793 and 873 K exhibited four distinct regimes in the variation of ultrasonic velocity with aging time. These different regimes have been correlated with the progressive evolution and coarsening of precipitate microstructure studied using TEM and microhardness measurements. The study revealed that ultrasonic velocity can be used to examine the secondary precipitation in the steel and the use of this technique as such can be extended to the health assessment of a component during service.     

Methods to overcome embrittlement problem in 9Cr–1Mo ferritic steel and its weldment

This article presents the issues that need to be addressed in ferritic steel, for their use in nuclear core, namely, the embrittlement and type IV cracking of weldment. It has been established that the ferritic steels possess a significantly higher resistance to radiation damage as compared to the present generation austenitic stainless steels and the creep behavior is satisfactory for applications up to 873 K. The major challenges that need to be addressed are the poor creep resistance of the weld joints and embrittlement of ferritic steels. This article describes the efforts taken at IGCAR to overcome the embrittlement problem by impurity control, grain boundary engineering or design of suitable thermomechanical treatments in a 9Cr–1Mo ferritic steel.     

Magnetic nondestructive evaluation of thermally degraded 2.25Cr–1Mo steel

Aging was performed to understand the microstructural degradation in 2.25Cr–1Mo steel. Microstructural parameters (mean equivalent carbide size, number of carbides per unit area), mechanical properties (UTS, Vickers hardness) and magnetic properties (coercivity, remanence) were measured to investigate the relationship among these parameters. The magnetic coercivity and remanence were observed to decrease rapidly in the initial 1000 h of aging time and then decrease slowly thereafter. Linear correlations between mechanical and magnetic properties were found.     

Identification of processing parameters for Fe–15Cr–2.2Mo–15Ni–0.3Ti austenitic stainless steel using processing maps

Abstract

The processing parameters for hot working of Fe–15Cr–2.2Mo–15Ni–0.3Ti austenitic stainless steel (alloy D9) are identified using processing maps developed on the basis of the dynamic materials model and hot compression data in the temperature range 850–1250°C and strain rate range 0.001–100 s^-1. The efficiency of power dissipation increased with increase in temperature and decrease in strain rate. Dynamically recrystallised microstructures resulted when the efficiency of power dissipation was in the range 27–37%, i.e. in the temperature range 1050–1250°C and strain rate range 0.001–0.5 s^-1. Flow localisation occurred in the regions of instability at temperatures lower than 1000°C and at higher strain rates. The dynamic recrystallisation regime observed in this alloy is compared with other austenitic stainless steels, namely, AISI type 304L and 316L.     

A study of breakaway oxidation of 9Cr–1Mo steel in a Hot CO2 atmosphere using Raman spectroscopy

Abstract

The microstructure of the oxide scale and parent metal in ferritic 9Cr–1Mo steel was observed to explore the oxidation and carburisation mechanisms upon exposure to a CO₂ gas environment at high temperature and high pressure. An experimental 9Cr–1Mo steel sample that had been oxidised at 580 °C for more than 165,000 hrs in coolant gas consisting primarily of CO₂ was analysed. To elucidate the oxidation characterisation, scanning Raman spectrometry was used to analyse the oxide close to the metal/oxide interface. Carbon was found to be deposited in the spinel layer. The microstructure and the distribution of elemental chemical composition were examined and analysed using optical and scanning electron microscopy combined with energy dispersive X-ray analysis. The results are discussed with relation to understanding the mechanisms of oxidation and carburisation which aim to underpin extension of the service life of components fabricated from this steel.     

Effect of microstructure on appearance of near-threshold fatigue fracture in Cr–Mo–V steel

Near-threshold fatigue crack growth behavior in 25Cr2NiMo1V steel with different microstructures was investigated by utilizing the load-shedding technique at ambient temperature. Crack surface morphology was observed by SEM with special emphases on the incidence of intergranular fracture and the influence on crack growth rates. Results show that the maximum intergranularity occurs at the ΔK corresponding to the cyclic plastic zone size being equivalent to the prior austenitic grain size. Two types of crack growth mode were observed in the near-threshold regime, i.e., the crystallographic mode of crack growth and the striation mode of crack advance. The incidence of faceted fracture was mainly rationalized by comparing the cyclic plastic zone size with the grain size. It is concluded that, in the crystallographic mode, lower crack growth rates in samples with higher heat treatment temperatures are caused by a greater degree of roughness-induced crack closure (RICC), faceted fracture induced crack closure (FFICC), and oxide-induced crack closure (OICC). The faceted fracture shows negligible influence on crack growth rates when cracks grow in a striation controlled mode.