Damage analysis in Fe–Cr–Ni centrifugally cast alloy tubes for reforming furnaces

Reformer furnaces tubes work under high temperature and pressure for a long time, which are very critical conditions for creep deformation and life of most common materials. Cast austenitic Fe–Cr–Ni alloys in the widely know HP grades are used for reformer tubes to allow a good service at temperatures that can be close to 1000 °C. This paper reports a study devoted to the damage analysis of reformer furnace tubes after more than 100,000 h of service. Tubes, made of a HP grade modified with Nb and Ti additions, were inspected in situ by a laser optic system to measure their internal diameter and evaluate creep deformation. With the aim of developing a criterion for deciding the substitution of components, samples of as cast material and samples, cut from the most deformed tubes put out of service, were considered to check changes of mechanical properties and metallurgical characteristics. Tensile and creep tests were carried out; moreover the metallographic observations included optical and scanning electron microscopy and energy dispersive X-ray microanalysis in order to measure locally the chemical composition.     

Dissolution of interdendritic σ phase in cast Ni–Fe–Cr alloy

Various sizes, fractions and morphologies of interdendritic σ phase in the as cast N08028 alloy due to different solidification conditions are characterised. Dissolution behaviours of the secondary phase in both the as cast and the forged alloys are investigated during heat treatment at 1100, 1150 and 1200°C. A recently developed analytical model, subjected to necessary modification, is applied to describe the dissolution process of σ phase in the alloys with and without prior hot deformation. A recipe derived from transformed fraction is applied to evaluate the effective activation energy for dissolution. It has been found that, the prior hot deformation accelerates the dissolution process, which can be attributed to the decreased particle size and the reduced effective activation energy.     

Effect of niobium on creep and creep crack growth of cast Ni–Cr austenitic steel

Abstract

An investigation of the effect of Nb on creep properties and creep crack growth rate in a 25Cr–35Ni–0·4C (wt-%) cast steel at 871 and 950°C was carried out. Tensile tests were also carried out at room temperature, 871, and 950°C. The tensile strength and elongation increased with an increase in Nb content at high temperatures. There existed an optimum Nb content for the creep properties and creep crack growth rate. Creep crack growth is controlled by creep deformation.

MST/1222     

Damage propagation mechanism in low-cycle creep fatigue of Cu–Cr–Zr alloy

This paper describes a characteristic damage propagation mechanism in low-cycle creep–fatigue of Cu–0.7Cr–0.09Zr (mass%), as investigated by creep–fatigue tests including strain controlled fatigue and stress-holding type creep, and following microstructural observations by scanning electron microscopy (SEM). The total stress-holding time until rupture in the creep–fatigue test was shorter than one-tenth of the rupture life in the simple creep test, and the rupture life of the specimen in the creep–fatigue test was shorter than half of that in the simple fatigue test. The SEM images suggest that the connection between fatigue crack propagating along grain boundaries and intergranular creep voids rapidly accelerates crack propagation.     

Hot ductility of a Fe–Ni–Co alloy in cast and wrought conditions

The hot ductility of Fe–29Ni–17Co alloy was studied in both cast and wrought conditions by hot tensile tests over temperature range of 900–1250 °C and at strain rates of 0.001–1 s⁻¹. Over the studied temperature range, the wrought alloy represented higher elongation and reduction in area as compared to the cast alloy. Dynamic recrystallization was found responsible for the higher hot ductility of the wrought alloy and the improvement of hot ductility of the cast alloy at high temperatures. At temperature range of 1000–1150 °C the wrought alloy exhibited a hot ductility drop while a similar trough was not observed in case of the cast alloy. It was also found that at temperatures of 1150–1250 °C the best hot ductility is achieved in both cases of cast and wrought alloy. The experimental data of flow stress were constitutively analyzed and the apparent activation energy of deformation was estimated to be 344 kJ/mol.     

Compressive and impression creep behavior of a cast Mg–Al–Zn–Si alloy

Creep behavior of an Mg–6Al–1Zn–0.7Si cast alloy was investigated by compression and impression creep test methods in order to evaluate the correspondence of impression creep results and creep mechanisms with conventional compression test. All creep tests were carried out in the temperature range 423–523 K and under normal stresses in the range 50–300 MPa for the compression creep and 150–650 MPa for impression creep tests. The microstructure of the AZ61–0.7Si alloy consists of β-Mg₁₇Al₁₂ and Mg₂Si intermetallic phases in the α-Mg matrix. The softening of the former at high temperatures is compensated by the strengthening effect of the latter, which acts as a barrier opposing recovery processes. The impression results were in good agreement with those of the conventional compressive creep tests. The creep behavior can be divided into two stress regimes, with a change from the low-stress regime to the high-stress regime occurring, depending on the test temperature, around 0.009 < (σ/G) < 0.015 and 0.021 < (σ_imp/G) < 0.033 for the compressive and impression creep tests, respectively. Based on the steady-state power-law creep relationship, the stress exponents of about 4–5 and 10–12 were obtained at low and high stresses, respectively. The low-stress regime activation energies of about 90 kJ mol⁻¹, which are close to that for dislocation pipe diffusion in the Mg, and stress exponents in the range of 4–5 suggest that the operative creep mechanism is pipe-diffusion-controlled dislocation viscous glide. This behavior is in contrast to the high-stress regime, in which the stress exponents of 10–12 and activation energies of about 141 kJ mol⁻¹ are indicative of a dislocation climb mechanism similar to those noted in dispersion strengthening mechanisms.     

Microstructural changes during annealing of cast Ni–Cr–Hf alloys

Abstract

In order to gain knowledge of the nickel–rich corner of the Ni–Cr–Hf phase diagram, microstructures of cast alloys and their evolution towards equilibrium conditions have been followed by optical and scanning electron microscopy, microprobe analysis, and quantitative metallography. The evolution of as–cast microstructures involves the development of a Ni₅Hf plate–like precipitate in two–phase alloys, and various morphological changes in three–phase alloys. As–cast structures are compared with those obtained by arc melting. Direct processing of the scanning electron microscope image has proved to be a valuable tool for microstructural characterization of the transforming phases.

MST/349     

Improvement of mechanical properties in severely plastically deformed Ni–Cr alloy

This study was carried out to evaluate the grain refining and mechanical properties in alloys that undergo severe plastic deformation (SPD). Conventional rolling (CR) and cross-roll rolling (CRR) were introduced as methods for SPD, and a Ni–20Cr alloy was selected as the experimental material. The materials were cold rolled to 90% thickness reduction and subsequently annealed at 700 °C for 30 min to obtain the fully recrystallized microstructure. The annealed materials after cold rolling were assessed through electron backscattered diffraction (EBSD) analysis to investigate the grain boundary characteristic distributions (GBCDs). The CRR process was more effective than the CR process in developing grain refinement; the grain size decreased from 70 μm in the initial material to 4.2 μm (CR) and 2.4 μm (CRR), respectively. The grain refinement affected mechanical properties such as microhardness, yield, and tensile strength, which were significantly increased relative to the initial material.     

Age hardening and creep resistance of cast Al–Cu alloy modified by praseodymium

The effects of praseodymium on age hardening behavior and creep resistance of cast Al–Cu alloy were investigated. The results indicated that praseodymium facilitated the formation of the θ′ precipitates during the age process and improved the hardness of the Al–Cu alloy. Besides, praseodymium resulted in the formation of the Al₁₁Pr₃ phase in the grain boundaries and among the dendrites of the modified alloy. Because of the good thermal stability of Al₁₁Pr₃ phase, it inhibits grain boundary migration and dislocation movement during the creep process, which contributes to the improvement in the creep resistance of the modified alloy at elevated temperatures.     

Analysis of material degradation and life assessment of 25Cr–38Ni–Mo–Ti wrought alloy steel (HPM) for cracking tubes in an ethylene plant

Radiant tubes made of wrought 25Cr–38Ni–Mo–Ti alloy steel (HPM) have been in-service for 76,500 h as cracking tubes in an ethylene plant and they are expected to provide reliable service for 100,000 h (11.4 years) or more. During service, the tube inner surfaces were operated at temperature in the range of 820–835 °C within which thermal cracking process occurred. These aged tubes were assessed to ensure continued safe operation. The assessment of material degradation was carried out using optical microscopy, scanning electron microscopy (SEM) in combination with energy dispersive X-ray (EDX) analysis, X-ray powder diffraction (XRD) analysis, Vickers microhardness measurement and stress rupture test to obtain stress–Larson–Miller parameter (LMP) curves for remaining life prediction. Results showed that microstructural degradation was observed at the inner surface of the radiant tubes marked by the damage of protective oxide film containing Cr₂O₃, Fe₂O₃ and SiO₂. Once this film was removed, carburization occurred and free C atoms involved during cracking of ethylene easily penetrated along austenitic grain boundaries. In addition, carbon diffusion into the tube metal seemed to promote precipitation of Cr₂₃C₆ at grain boundaries and within the grains resulting in a sharp increase in hardness. The outer surface of the radiant tubes, on the other hand, was exposed to higher temperature, typically 1040–1100 °C during operation and creep damage seemed to be the main cause of material degradation. Based on stress rupture test, the remaining life of the radiant tubes is expected to be 21,107 h (2.4 years) consistent with the design life. In the present investigation, factors affecting creep are discussed.     

Tensile creep behavior of Sn–Ag–Cu–Ni multicomponent lead-free solder alloy

In the process of electronic packaging, the dissolution of under bump metallizations, such as Cu and Ni, into liquid solder occurs during soldering, which can change the original solder to a multicomponent one. Under the trend of miniaturization, it is quite necessary to evaluate the properties of multicomponent solder with excessive Cu and Ni compositions. In this study, the tensile creep behavior of Sn–3.5Ag–2.0Cu–0.5Ni multicomponent lead-free solder alloy is investigated at three temperatures, i.e., 303, 348 and 393 K. The steady-rate creep rates are obtained in the range of 10^?4–10^?8 s^?1, when the normalized stress, σ/E, is in the range of 10^?4–10^?3. Based on the Dorn equation, the apparent stress exponent (n _a), threshold stress (σ _th), and activation energy of creep (Q _C) are calculated at the three temperatures. It is found that the Sn–3.5Ag–2.0Cu–0.5Ni solder alloy shows a better creep performance than pure tin and eutectic Sn–3.5Ag solder due to the strengthening effect of Ag₃Sn and (Cu,Ni)₆Sn₅ IMC precipitations. The true stress exponent for creep is identified to be 7, indicating that the creep behave is controlled by the dislocation-pipe diffusion in the tin matrix.     

Thermomechanical processing of Cu–Ni–Si–Cr–Mg alloy

Abstract

The relationships between the structure and properties of a Cu–Ni–Si–Cr–Mg alloy are discussed. Possible methods of improving the properties and operating characteristics of semiproducts manufactured from this type of alloy were investigated. It was found that these properties, in particular their stability, depend mainly on the structure of the material, which in turn depends on the thermomechanical treatment. Examples and possible applications are presented.

MST/1436     

Oxidation behaviour of nanocrystalline Fe–Ni–Cr–Al alloy coatings

Abstract

Nanocrystalline Fe–Ni–Cr–Al alloy coatings with ～4 wt-%Al were produced using the unbalanced magnetron sputter deposition technique with a composite 310S stainless steel target embedded with aluminium plugs. The oxidation behaviour of the coatings was studied, during which complete external α-Al₂O₃ scales were formed. During isothermal oxidation tests at 950, 1000, and 1050°C, the oxidation kinetics followed an essentially parabolic rate law, and the oxidation constants were measured to be 2·06 × 10^-3, 4·23 × 10^-3, and 1·14 × 10^-2 mg² cm^-4 h^-1 respectively. During a cyclic oxidation test at 1000°C the α-Al₂O₃ scale showed good scale spallation resistance. The surface hardness of the coatings was measured with a Knoop indentor before and after oxidation. After oxidation, the coating surface hardness was still significantly higher than that of the uncoated specimen, demonstrating the potential this coating has in the improvement of high temperature erosion resistance.     

Microstructure and properties of sintered Cu–25Cr alloy

Abstract

Sintered and precipitation hardened Cu–25Cr (wt-%) contact alloys were prepared and their properties related to those of a precipitation and strain hardened reference alloy. The evolution of microstructure during sintering, solution heat treatment, and precipitation hardening was studied, in particular with respect to precipitate morphology and growth. The influence of microstructure on the hardness, strength, and electrical conductivity of Cu–25Cr alloys was evaluated. The relative importance of precipitation and strain hardening has been clarified, and it is shown that the contribution of the precipitation effect is dominant. The importance of monitoring the evolution of microstructure with respect to long term stability of Cu–Cr contact alloys is emphasised.

MST/999     

Nitriding of Co–Cr–Mo alloy in nitrogen

Using the results of a thermodynamic analysis, a Co–Cr–Mo alloy was successfully nitrided in nitrogen at temperatures of 1073–1473 K. The near-surface microstructure of the treated Co–Cr–Mo alloy was characterized using X-ray diffraction, field-emission scanning electron microscopy, electron probe micro-analyzer, and transmission electron microscopy equipped with energy-dispersive X-ray spectroscopy. The results indicated that the highest nitriding efficiency was achieved at the treatment temperature of 1273 K, with the size and coverage of the nitride particles on sample's surface increasing with an increase in the treatment duration. After nitriding at 1273 K for 2 h, numerous nitride particles, consisting of an outer Cr₂N layer and an inner π phase layer, were formed on top of the nitrogen-containing γ phase, and some π phase also precipitated in the alloy matrix at the sub-surface level.     

Effect of σ-Phase on the creep properties of Cr25Ni20 stainless steel

It is concluded from above that effect of σ-phase on creep properties depends on particle size and distribution. Fine σ-phase particles dispersively precipitated along grain boundaries and within grains increase creep resistance and rupture strength, having general characteristics of dispersion hardening.     

The effect of heat treatments on the creep–rupture properties of a wrought Ni–Cr heat-resistant alloy at 973 K

The effect of heat treatments on the creep–rupture properties was investigated on a wrought Ni–Cr heat-resistant alloy at 973 K. Short-time aging (aging for 3.6 ks (1 h) at 973 K) was made on the solution-treated specimens with different grain sizes. The fine-grained specimen (the grain diameter, d = 45.2 μm) produced by short-time solution treatment exhibited almost the same rupture life and superior creep ductility as those of the medium-grained specimen (d = 108 μm) produced by normal solution treatment. The fine-grained specimen and medium-grained specimen showed the longer rupture life compared with the specimen with recommended aging. The principal strengthening of specimens was attributed to the precipitation hardening by γ′ phase particles. The fine-grained specimen had the highest hardness, and the increase of the hardness was observed in both the fine-grained and the medium-grained specimens during creep at 973 K. However, coarse-grained specimen (d = 286 μm) with high-temperature long-time solution treatment exhibited significantly short rupture life owing to insufficient precipitation hardening after the short-time aging and during creep. Ductile intergranular fracture with dimples occurred in the fine-grained specimen, while brittle intergranular fracture was observed in the medium-grained specimen and in the specimen with recommended aging. Both transgranular fracture and brittle intergranular fracture were observed in the coarse-grained specimen. A simple heat treatment composed of short-time solution treatment and short-time aging is applicable to high-temperature components of wrought Ni–Cr alloys.     

Grain boundary precipitation strengthening in high temperature creep of Fe15Cr25Ni alloys

Grain boundary carbide precipitation gives rise to a dramatic decrease in creep rates compared with those of a single phase alloy. The high stress exponent (n=7) and creep activation energy (Q_C > Q_sd) have been found due to these intergranular carbides, indicating that they both increase creep resistance and change creep characteristics of alloys. The model present here rationalizes the observed behavior in single phase and two phase alloys with grain boundary carbides by a unified power law equation involving boundary obstacle stress. The predictions of this model are in close agreement with experimental results.     

Compressive creep behaviour of Mg–Li–Al alloy

Abstract

The compressive creep behaviour of as cast Mg–14Li–1·3Al (wt-%) alloy was investigated in the temperature range of 20?85°C and under different compressive stress in the range of 37·3–74·6 MPa with special apparatus. Primary creep deformation and steady creep rate increase with temperature and applied stress. The compressive creep behaviour obeys an empirical equation ln t=C?nln σ + Q/RT, where t is the time to a selected creep strain, σ is the applied stress, T is the absolute temperature, R is the gas constant, and C, n, and Q are constants for the experimental alloy. The average values of the exponent n and the creep activation energy Q are 4·33 and 101·13 kJ mol^?1 respectively. The creep rate controlling mechanism is the dislocation climb and the lattice diffusion of Li in the experimental alloy under the testing conditions.