Effect of quenching,tempering, and cold rolling on creep deformation behavior of a tempered martensitic 9Cr-1W steel

The effect of quenching, tempering, cold-rolling, and aging treatments, which produce different dislocation substructures and different carbide distributions, on the creep-deformation behavior is investigated for a tempered martensitic 9Cr-1W steel at 873 K, mainly. The creep rate vs time curves indicate transient creep, where the creep rate decreases with time, and accelerating creep, where the creep rate increases with time. The minimum creep rate is closely correlated with the onset time of acceleration creep and is inversely proportional to the duration of the transient creep region. The onset of acceleration creep shifts to shorter times for the specimens subjected to the quenching, 20-hour tempering (long-term tempering) at 1023 K, and cold-rolling treatments than that for the specimen subjected to the standard quenching and tempering (QT) treatment. The onset of acceleration creep is closely correlated with the migration of lath or subgrain boundaries, causing the coarsening of laths or subgrains. Dislocation cells produced by cold rolling are free of M₂₃C₆ carbides. The migration and recovery of dislocation cells significantly promote the onset of acceleration creep. The preferential distribution of M₂₃C₆ carbides along lath boundaries is effective for the retardation of the onset of acceleration creep for up to longer times by the stabilization of lath boundaries. In the acceleration creep region, after reaching a minimum creep rate, the logarithm of the creep rate increases linearly with strain for a wide range of strains. The time to rupture (tr) is inversely proportional to the minimum creep rate times the acceleration of the creep rate (d ln /dε) in the acceleration creep region, but is not proportional to only the minimum creep rate, as given by

Investigation of precipitation behavior in a weld deposit of 11Cr-2W ferritic steel

This article is aimed at investigating the difference in precipitation behavior in the fine-grained heat-affected zone (FGHAZ), coarse-grained heat-affected zone (CGHAZ), and base metal for the welded joint of high Cr ferritic heat-resistant steel (11Cr-0.4Mo-2W-1Cu-V-Nb, normalized 1323 K×1 h and tempered 1033 K×1 h). Simulated HAZ (SHAZ) specimens were used, whose thermal cycles were controlled to be the same as those in the actual welded joint with peak temperatures of 1523 and 1173 K to represent CGHAZ and FGHAZ, respectively. Based on scanning electron microscopy (SEM) observation, it looks that the precipitates in FGHAZ specimens (1173 K) were fewer and larger than those in CGHAZ (1523 K) specimens and base metal specimens. This phenomenon implied that the growth and coarsening of precipitates in FGHAZ may play a role in the deterioration of creep properties and type IV cracking, which was observed in previous creep tests. X-ray diffraction analysis for the electrolytic extraction showed that the types of precipitates are the same for the 1173 K specimens and base metal specimens, including M₂₃C₆, MX, Laves phase, and μ phase. Further, the elemental analysis of the extraction showed that the mass percentages of Cr, W, and Mo in the precipitates to specimen mass were higher in the FGHAZ specimen than those in the base metal specimen, especially during the period between 600 and 2464 hours. Finally, a two-dimensional (2-D) model was proposed to simulate the precipitation behavior of the Laves phase.     

9Cr低活化马氏体钢高温变形行为

采用Gleeble-1500D热模拟试验机研究了9Cr低活化马氏体钢在950~1200℃、应变速率为10^-2~10s^-1变形条件下的热压缩变形行为,并用金相显微镜观察了相应显微组织的变化.回归分析得出在0.15~0.8真应变量范围内变形激活能和材料常数随真应变量变化的关系式,并得出双曲正弦本构方程;利用数学方法直接从真应力-真应变曲线获得动态再结晶的峰值应力、临界应力、峰值应变和临界应变;回归得出了峰值应力、临界应力、峰值应变、临界应变和动态再结晶晶粒大小与Zener-Hollomon参数的关系式.     

Effect of normalization temperature on the creep strength of modified 9Cr-1Mo steel

The effect of normalization temperature from 850 °C to 1050 °C on the structure and creep-rupture properties of modified 9Cr-1Mo steel was studied. Normalization at temperatures below 925 °C resulted in structures containing significant polygonized, recovered ferrite. The ferrite structures had poor creep-rupture strength: roughly two orders of magnitude increase in minimum creep rate or decrease in rupture life for 850 °C compared to 1050 °C normalization at test conditions of 600 °C and 145 MPa. Room-temperature strength and hardness were also reduced. The microstructure after normalization at the standard 1050 °C temperature consisted of tempered martensite with fine M₂₃C₆ carbide along prior austenite and lath boundaries and fine MX carbonitride precipitates within the laths. Normalization at temperatures between 925 °C and 1000 °C also resulted in reduced creep strength in comparison with 1050 °C normalization, even though tempered martensite microstructures were formed and little change in room-temperature strength was observed; the reduction was attributed to subtle differences in the MX precipitates. The effect of reduced normalization temperature was more pronounced for higher-temperature, lower-stress creep-rupture conditions.     

Heat treatment effects on creep and rupture behavior of annealed 2.25 Cr-1 Mo steel

The strength of 2 1/4 Cr-1 Mo steel depends on the microstructure, which, in turn, de-pends on the heat treatment. In the fully annealed and isothermally annealed conditions, the microstructure is primarily proeutectoid ferrite with varying amounts of bainite and pearlite. The relative amounts of the latter constituents depend on the cooling rates during the anneal. The creep and rupture properties were determined for steel plates (from a single heat) given three different annealing treatments: two were fully annealed, but cooled at different rates from the austenitizing temperature, and the third was iso-thermally annealed. Properties were determined at 454, 510, and 566°C. At 454 and 510°C, the cooling rate had a significant effect on the creep and rupture properties, with the ma-terial cooled fastest being the strongest. Although at 510°C strengths at short rupture times differed widely, the properties approached a common value at longer rupture times. The properties differed very little at 566°C, even for short rupture times. The effect of heat treatment was concluded to be the result of interaction solid solution hardening, a dislocation-drag process. This process gave rise to nonclassical creep curves (as op-posed to classical curves with single primary, secondary, and tertiary stages). By examining the creep-curve shape, it was possible to interpret the heat treatment effects on the creep-rupture properties.     

Comprehensive microstructural characterization in modified 9Cr-1Mo ferritic steel by ultrasonic measurements

Modified 9Cr-1Mo ferritic steel (T91/P91) has been subjected to a series of heat treatments consisting of soaking for 5 minutes at the selected temperatures, starting from the α-phase region (1073 K) to the γ + δ-phase region (1623 K), followed by oil quenching. Hardness measurements, microstructural features, and grain-size measurements by the linear-intercept method have been used for correlating them with the ultrasonic parameters. Ultrasonic velocity and attenuation measurements, and spectral analysis of the first backwall echo have been used for characterization of the microstructures obtained by various heat treatments. As the soaking temperature increased above Ac ₁, the ultrasonic velocity decreased because of the increase in the volume fraction of martensite in the structure. There were sharp changes in the ultrasonic velocities corresponding to the two critical temperatures, Ac ₁ and Ac ₃. Ultrasonic longitudinal- and shear-wave velocities were found to be useful in identifying the Ac ₁ and Ac ₃ temperatures and for the determination of hardness in the intercritical region. However, ultrasonic attenuation and spectral analysis of the first backwall echo were found to be useful to characterize the variation in the prior-austenitic grain size and formation of δ ferrite above the Ac ₄ temperature. The scattering coefficients have been experimentally determined for various microstructures and compared with the theoretically calculated value of the scattering coefficients for iron reported in literature.     

Fe-13Cr-5Ni马氏体不锈钢在连续加热过程中两相区的奥氏体生长行为

通过光学显微镜、透射电子显微镜、X射线衍射仪以及显微硬度仪研究Fe-13Cr-5Ni马氏体不锈钢在加热过程中的组织转变行为.结果表明,Fe-13Cr-5Ni钢在10℃·s^-1的加热速率下,加热至奥氏体单相区,冷却至室温后具有明显的“组织遗传冶现象.奥氏体以“针状冶形式在马氏体板条界处形核并沿着马氏体板条界长大,与母相间保持Kurdjumov-Sachs （K-S）位向关系.加热至两相区不同温度然后淬火至室温,奥氏体的量随两相区保温温度的升高先增加再减少,650℃时对应室温下残余奥氏体的极大值,并且这一变化趋势与试样显微硬度测试结果所得结论一致.     

Effects of aluminum content on the mechanical properties of a 9Cr-0.5Mo-1.8W steel

The effects of aluminum content on mechanical properties of a 9Cr-0.5Mo-1.8W steel have been investigated. It was found that aluminum addition had a beneficial effect on toughness, but significantly reduced the creep resistance of the steel, especially on the long-term side. Examination of the microstructure and precipitation characteristics revealed that almost all of the aluminum added existed as AIN-type nitrides after normalizing and tempering. The undissolved AIN in high aluminum steels resulted in a dramatic refinement of prior austenite grains, which contributed to the improvement of toughness and was also partially responsible for the decreased creep rupture strength. The formation of AIN suppressed the precipitation of VN-type nitride; AIN also provided formation sites for Nb(C, N) and M₂₃C₆ type, which had an equivalent effect to the coalescence of these precipitates on AIN, resulting in the reduction of precipitate density and, therefore, decreased creep resistance.     

Microstructural characterization of 5 to 9 pct Cr-2 pct W-V-Ta martensitic steels

The microstructure of 9Cr-2W-0.25V-0.1C (9Cr-2WV), 9Cr-2W-0.25V-0.07Ta-0.1C (9Cr-2WVTa), 7Cr-2W-0.25V-0.07Ta-0.1C (7Cr-2WVTa), and 5Cr-2W-0.25V-0.07Ta-0.1C (5Cr-2WVTa) steels (all compositions are in wt pct) have been characterized by analytical electron microscopy (AEM) and atom probe field ion microscopy (APFIM). These alloys have potential applications in fusion reactors because they exhibit reduced neutron activation in comparison to the conventional Cr-Mo steels. The matrix in all four alloys was 100 pct martensite. The precipitate type in the steels depended primarily on the chromium level in the alloy. In the two 9Cr steels, the stable phases were blocky M₂₃C₆ and small spherical precipitates previously identified as MC. The two lower-chromium steels contained blocky M₇C₃ and small needle-shaped carbonitrides in addition to M₂₃C₆. The AEM and APFIM analyses revealed that, in the steels containing tantalum, the majority of the tantalum was in solid solution. With the exception of a few of the small spherical precipitates in low-number densities in the 9Cr-2WVTa, none of the other precipitates contained measurable tantalum. The experimentally observed phases were in agreement with those predicted by phase equilibria calculations using the ThermoCalc software. However, a similar match between the experimental and predicted values of the phase compositions did not occur in some instances. Atom probe analyses directly confirmed the crucial role of trace amounts of nitrogen in the formation of vanadium-rich carbonitrides as predicted by thermodynamic equilibrium calculations.     

The role of coincidence-site-lattice boundaries in creep of Ni-16Cr-9Fe at 360 °C

The objective of this study is to understand and quantify the role of the coincidence-site-lattice boundary (CSLB) population on creep deformation of Ni-16Cr-9Fe at 360 °C. It is hypothesized that an increase in the CSLB population decreases the annihilation rate of dislocations in the grain boundary, leading to an increase in the internal stress and a decrease in the effective stress. The result is a reduction in the creep strain rate. The role of CSLBs in deformation is, thus, to increase the internal stress by trapping run-in lattice dislocations at the grain boundaries as extrinsic grain boundary dislocations (EGBDs), creating backstresses on following dislocations rather than annihilating them, as in the case of high-angle boundaries (HABs). The hypothesis was substantiated by showing (1) that dislocation absorption kinetics differ substantially between a CSLB and an HAB, and (2) that the CSLB fraction strongly affects the internal stress in the solid. Dislocation absorption kinetics were measured by comparing EGBD density in transmission electron microscopy (TEM). Results showed that CSLBs contain an EGBD density which is 3 times higher than HABs at 1.25 pct strain. Internal stress was measured by the stress dip test and was found to be ≈ 30 MPa higher in the CSLB-enhanced sample. Steady-state creep rates of Ni-16Cr-9Fe in 360 °C argon were also found to be strongly affected by the grain boundary character distribution. Increasing the CSLB fraction by approximately a factor of 2 resulted in a decrease in steady-state creep rates by a factor of 8 to 26 in coarse-grain (330 μm) samples and a factor of 40 to 66 in small-grain (35 μm) samples. It is postulated that annihilation of EGBDs only occurs at triple lines where at least two HABs intersect. By using a geometric relationship to evaluate the probability of EGBDs annihilating at a triple line, the model predicts a non-linear dependence of the creep rate with CSLB fraction, yielding excellent correlation with measurement. The model provides a physical basis for measurements which show that increasing the CSLB fraction by only moderate amounts can greatly reduce the steady-state creep rate in Ni-16Cr-9Fe.     

Dislocation damping and microstructural evolutions during creep of 2.25Cr-1Mo steels

We studied the microstructural evolution of 2.25Cr-1Mo steels subjected to tensile creep at 923 K through monitoring of shear-wave attenuation and velocity, using electromagnetic acoustic resonance (EMAR). Contactless transduction based on the magnetostrictive mechanism is the key to establishing a monitor for microstructural change in the bulk of the metals with a high sensitivity. In the short interval, 50 to 60 pct of the creep life, attenuation experiences a peak, being independent of the applied stress. This novel phenomenon is interpreted in terms of the drastic change in dislocation mobility and rearrangement, which is supported by transmission electron microscopy (TEM) observations for dislocation structure. At this particular period, the dense dislocation structure starts to transform to subgrain boundaries, which temporally accompanies long, free dislocation, absorbing much ultrasonic energy to produce the attenuation peak. The EMAR has the potential to assess the damage advance and to predict the remaining creep life of metals.     

Ball-indentation test technique for evaluating thermal and creep damage of modified 9Cr-1Mo steel

The Ball-Indentation (BI) testing based on multiple cycles of loading-unloading using a spherical indenter is a useful technique for evaluating tensile properties from a very small volume of material. In this study, the BI technique has been used in a novel way to evaluate the changes in mechanical properties of Modified (Mod) 9Cr-1Mo caused by creep exposures. Microstructural degradation of varying degrees in Mod 9Cr-1Mo steel is simulated by conventional creep test terminated at various strains. By carrying out BI tests on unstressed head and stressed gage portions of the creep specimens, the changes in the strength and ductility are evaluated. Microstructural evolution in the creep exposed conditions studied using transmission electron microscopy is related to the strength changes caused by the stressed exposures.     

Creep-rupture behavior of forged, thick section 9Cr-1Mo ferritic steel

Detailed investigations have been performed to examine the creep-rupture behavior of a 1000-mm diameter and 300-mm-thick tube plate forging of 9Cr-1Mo ferritic steel in quenched and tempered (Q + T), simulated postweld heat treatment (SPWHT), and thermally aged (TA) conditions. Creep tests were conducted over a wide stress range (50 to 275 MPa) at 793 and 873 K. The alloy exhibited well-defined primary, steady-state, and extended tertiary creep stages at all test conditions. At 793 K, no significant difference in the creep-rupture properties was noted between Q + T, SPWHT, and TA conditions. On the other hand, SPWHT specimens exhibited lower creep-rupture strength than that of Q + T specimens at 873 K. Applied stress (σ _a ) dependence of rupture life (t _r ) exhibited two-slope behavior. Both the Monkman-Grant (ε _s .t _r = C _MG) and modified Monkman-Grant (ε _s .t _r /ε _f = C _MMG) relationships were found to be valid for 9Cr-1Mo steel, where ε _s is the steady-state creep rate and ε _f is the strain to failure. The two-slope behavior was also reflected as two constants in the Monkman-Grant relationship (MGR) and modified Monkman-Grant relationship (MMGR) in the two stress regimes. Further, two creep damage tolerance factors (λ = 1/C _MMG) of 5 and 10 were also observed in the high and low stress regimes, respectively. The alloy exhibited high creep ductility, which was retained for longer rupture lives at low stresses, and the creep ductility increased with increase in test temperature. The failure mode remained trangranular under all test conditions. The extensive tertiary creep in the alloy has been attributed to microstructural degradation associated with precipitates and dislocation substructure. The creep-rupture strength of the forging was found to be lower than that of thin section bars and tubes.     

Low cycle fatigue properties of modified 9Cr-1Mo ferritic martensitic steel weld joints in sodium environment

Mod.9Cr-1Mo ferritic-martensitic steel is the material chosen for the steam generator of the Prototype Fast Breeder Reactor being built at Kalpakkam, India. The use of sodium as a heat transfer medium for Liquid Metal Fast Breeder Reactors (LMFBRs) necessitates a comprehensive understanding of the effects of dynamic sodium on the Low Cycle Fatigue (LCF) behaviour of structural components. Moreover welds being the weak links in any structure, it is necessary to evaluate the LCF behaviour of joints in sodium environment, more so in Mod.9Cr-1Mo steel because of the well established Type — IV cracking in this material. With this aim in view, a programme has been initiated to evaluate the LCF properties of weld joints of this steel in dynamic sodium environment. A facility has been developed in-house for mechanical property evaluation in dynamic sodium. LCF tests conducted in flowing sodium environment at 823 and 873 K showed a similar trend in cyclic stress response in air and sodium environments exhibiting a continuous cyclic softening behaviour. The fatigue lives are significantly improved in sodium environment when compared to the data obtained under identical testing conditions in air environment. The lack of oxidation in sodium environment is considered to be responsible for the delayed crack initiation and consequent increase in fatigue life. Comparison with RCC-MR code shows that the design curve based on air tests is conservative.     

Precipitation of Fe2W laves phase and modeling of its direct influence on the strength of a 12Cr-2W steel

Precipitation of Fe₂W Laves phase in a 12Cr-2W power plant steel is investigated by using transmission electron microscopy (TEM). Fe₂W Laves phase is found to be coherent with the matrix and has a stacking fault structure. The influence of formation of Fe₂W Laves phase on the yield strength of the steel is quantitatively evaluated. The modeling result indicates that the strengthening effect from the formation of Laves phase particles is diminished by the loss of solid solution strengthening of alloying elements, and, as a result, the strength of the steel remains similar. The effect of clustering and coarsening of Laves precipitates on the strength of the steel is also studied. It is showed that clustering and coarsening decreases the strengthening effect of Laves phase. The limitation of the modeling approach currently adopted is also discussed.     

Interesting relationships for creep deformation and damage and their applicability for 9Cr-1Mo ferritic steel

The paper presents the validity of several interesting relationships examined for better understanding of creep behaviour of 9Cr-1Mo ferritic steel. Creep rate-rupture time relationships of Monkman-Grant type have been found to be valid. Like stress dependence of creep rate and rupture life, both Monkman-Grant and modified Monkman-Grant relations (MGR and MMGR) exhibited distinct constant values of C _MG and C _MMG , respectively for low and high stress regimes. The validity of MGR and MMGR is a consequence of the creep deformation behaviour of 9Cr-1Mo ferritic steel obeying first order kinetics. On the basis of creep rate-rupture time relationships of Monkman-Grant type, several other relationships involving transient and tertiary creep parameters have been evolved and their applicability have been examined for the steel. Analogous to MGR and MMGR, a relationship involving transient creep parameters and the other involving tertiary creep parameters were found to be valid. Further, 9Cr-1Mo steel obeyed a recently introduced critical damage criterion interrelating time to reach Monkman-Grant ductility with rupture life, and the criterion depends only on creep damage tolerance factor. This unique relationship is evolved based on the seminal concept of time to reach Monkman-Grant ductility as the time at which the useful safe creep life is exhausted and damage attains a critical level. The important implications of this concept have been discussed.     

Effect of fine precipitation and subsequent coarsening of Fe<Subscript>2</Subscript>W laves phase on the creep deformation behavior of tempered martensitic 9Cr-W steels

The effect of fine precipitation and subsequent coarsening of Fe₂W Laves phase on the creep deformation behavior was investigated for simple 9Cr-W steels containing 0, 1, 2, and 4 wt pct W. After tempering, the specimens were subjected to creep tests at 823, 873, and 923 K for up to 15,000 hours. The precipitation of Fe₂W Laves phase takes place during creep at boundaries from the supersaturated solid solution of the high-W steels, the 9Cr-2W and 9Cr-4W steels, but not in the low-W steels, the 9Cr-0W and 9Cr-1W steels. The fine precipitation of Fe₂W Laves phase decreases the creep rate in the primary or transient creep region, while the subsequent large coarsening of Fe₂W Laves phase reduces the precipitation strengthening and promotes the acceleration of creep rate in the tertiary or acceleration creep region after reaching a minimum creep rate. The change in shape of creep rate curves with stress and temperature is explained by taking fine precipitation and subsequent coarsening of Fe₂W Laves phase into account.     

Effect of initial microstructure on microstructural instability and creep resistance of XD TiAl alloys

A number of lamellar structures were produced in XD TiAl alloys (Ti-45 at. pct and 47 at. pct Al-2 at. pct Nb-2 at. pct Mn+0.8 vol pct TiB₂) by selected heat treatments. During creep deformation, microstructural degradation of the lamellar structure was characterized by coarsening and spheroidization, resulting in the formation of fine globular structures at the grain boundaries. Grain boundary sliding (GBS) was thought to occur in local grains with a fine grain size, further accelerating the microstructural degradation and increasing the creep rate. The initial microstructural features had a great effect on microstructural instability and creep resistance. Large amounts of equiaxed γ grains hastened dynamic recrystallization, and the presence of fine lamellae increased the susceptibility to deformation-induced spheroidization. However, the coarsening and spheroidization were suppressed by stabilization treatments, resulting in better creep resistance than the microstructures without these treatments. Furthermore, well-interlocked grain boundaries with lamellar incursions were effective in restraining the onset of GBS and microstructural degradation. In the microstructures with smooth grain boundaries, a fine lamellar spacing significantly lowered the minimum creep rate but rapidly increased the tertiary creep rate for the 45 XD alloy. For the 47 XD alloy, well-interlocked grain boundaries dramatically improved the creep resistance of nearly and fully lamellar (FL) structures, in spite of the presence of coarse lamellar spacing or equiaxed γ grains. However, it may not be feasible to produce a microstructure with both a fine lamellar spacing and well-interlocked grain boundaries. If that is the case, it is suggested that the latter feature is more beneficial for creep resistance in XD TiAl alloys with relatively fine grains.     

The effect of ageing on the ductility of 9Cr-1 Mo steel

A study has been made of the effects of ageing at 550°C on the ductility and fracture mechanisms in a 9 Cr-1 Mo steel. Although the fracture mode remains ductile, ageing at times up to 5000 h causes a progressive reduction in ductility. Voids are nucleated at both coarsely distributed inclusions and at much more finely distributed precipitates, and the principal effect of ageing is to enhance void formation at precipitates. This enhancement is due to a combination of phosphorus segregation to carbide precipitate-matrix interfaces and, after ageing for 5000 h, to the precipitation of Fe₂Mo (Laves phase). An important aspect of the observations is that void nucleation at precipitates occurs continuously with increasing strain until failure occurs and the results are consistent with a failure criterion based on the achievement of a critical void spacing.