Carbon Redistribution and Carbide Precipitation in a High-Strength Low-Carbon HSLA-115 Steel Studied on a Nanoscale by Atom Probe Tomography

HSLA-115 is a newly developed Cu-bearing high-strength low-carbon martensitic steel for use in Naval structural applications. This research provides, for the first time, a comprehensive compositional analysis of carbon redistribution and associated complex phase transformations in an isothermal aging study of HSLA-115 at 823 K (550 °C). Specifically, we characterize carbon segregation at lath boundaries, grain-refining niobium carbonitrides, cementite, and secondary hardening M₂C carbides, in addition to copper precipitation, by 3D atom probe tomography (APT). Segregation of carbon (3 to 6 at. pct C) is observed at martensitic lath boundaries in the as-quenched and 0.12-hour aged microstructures. On further aging, carbon redistributes itself forming cementite and M₂C carbides. Niobium carbonitride precipitates do not dissolve during the austenitizing treatment and are inherited in the as-quenched and aged microstructures; these are characterized along with cementite by synchrotron X-ray diffraction and APT. Sub-nanometer-sized M₂C carbide precipitates are observed after the formation of Cu precipitates, co-located with the latter, indicating heterogeneous nucleation of M₂C. The temporal evolution of the composition and morphology of M₂C carbides at 823 K (550 °C) is described using APT; their precipitation kinetics is intertwined with Cu precipitates, affecting the bulk mechanical properties of HSLA-115. Phase compositions determined by APT are compared with computed compositions at thermodynamic equilibrium using ThermoCalc.     

Reverse Shape Memory Effect Related to α → γ Transformation in a Fe-Mn-Al-Ni Shape Memory Alloy

In this study, we investigated the shape memory behavior and phase transformations of solution-treated Fe_43.61Mn_34.74Al_13.38Ni_8.27 alloy between room temperature and 1173 K (900 °C). This alloy exhibits the reverse shape memory effect resulting from the phase transformation of α (bcc) → γ (fcc) between 673 K and 1073 K (400 °C and 800 °C) in addition to the shape memory effect resulting from the martensitic reverse transformation of γ′ (fcc) → α (bcc) below 673 K (400 °C). There is a high density of hairpin-shaped dislocations in the α phase undergoing the martensitic reverse transformation of γ′ → α. The lath γ phase, which preferentially nucleates and grows in the reversed α phase, has the same crystal orientation with the reverse-transformed γ′ martensite. However, the vermiculate γ phase, which is precipitated in the α phase between lath γ phase, has different crystal orientations. The lath γ phase is beneficial to attaining better reverse shape memory effect than the vermiculate γ phase.     

Comparison of shape memory characteristics of a Ti-50.9 At. Pct Ni alloy aged at 473 and 673 K

The effect of aging on transformation and deformation behavior, i.e., the transformation temperatures, shape memory behavior, and multistage martensitic and R-phase transformations, was investigated for a Ti-50.9 at. pct Ni alloy aged at a low temperature (<600 K) rarely used for practical applications and at a high temperature (>600 K) conventionally used for practical applications. It was found that there are many differences between aging at 473 and 673 K. The martensitic and R-phase transformation temperatures significantly varied depending on aging time and temperature. It is found that two-stage R-phase and multistage martensitic transformations appear in both the specimens aged at 473 and 673 K, respectively. The two-stage R-phase transformation appeared by aging at 473 K over 36 ks, while the multistage martensitic transformation (MSMT) appeared by aging at 673 K in the range of aging times between 1.2 and 36 ks. It is found that the critical stress for slip increases with increasing aging time in specimens aged at 473 K, while that of specimens aged at 673 K increases with increasing aging time until reaching a maximum, then it decreases with a further increase in aging time. It is also found that the critical stress for slip is superior for specimens aged at 473 K than that for specimens aged at 673 K. It was confirmed that dense and fine lenticular precipitates of about 10 nm in length were formed through aging, resulting in superior shape memory characteristics.     

Effects of Aging Temperature on Electrical Conductivity and Hardness of Cu-3 at. pct Ti Alloy Aged in a Hydrogen Atmosphere

To improve the balance of the electrical conductivity and mechanical strength for dilute Cu-Ti alloys by aging in a hydrogen atmosphere, the influence of aging temperature ranging from 673 K to 773 K (400 °C to 500 °C) on the properties of Cu-3 at. pct Ti alloy was studied. The Vickers hardness increases steadily with aging time and starts to fall at 3 hours at 773 K (500 °C), 10 hours at 723 K (450 °C), or over 620 hours at 673 K (400 °C), which is the same as the case of conventional aging in vacuum. The maximum hardness increases from 220 to 236 with the decrease of aging temperature, which is slightly lower than aging at the same temperature in vacuum. The electrical conductivity at the maximum hardness also increases from 18 to 32 pct of pure copper with the decrease of the temperature, which is enhanced by a factor of 1.3 to 1.5 in comparison to aging in vacuum. Thus, aging at 673 K (400 °C) in a hydrogen atmosphere renders fairly good balance of strength and conductivity, although it takes nearly a month to achieve. The microstructural changes during aging were examined by transmission electron microscopy (TEM) and atom-probe tomography (APT), and it was confirmed that precipitation of the Cu₄Ti phase occurs first and then particles of TiH₂ form as the third phase, thereby efficiently removing the Ti solutes in the matrix.     

Stability of Ni3(Al,Ti) Gamma Prime Precipitates in a Nickel-Based Superalloy Inconel X-750 Under Heavy Ion Irradiation

Phase stability of Ni₃(Al, Ti) precipitates in Inconel X-750 under cascade damage was studied using heavy ion irradiation with transmission electron microscope (TEM) in situ observations. From 333 K to 673 K (60 °C to 400 °C), ordered Ni₃(Al, Ti) precipitates became completely disordered at low irradiation dose of 0.06 displacement per atom (dpa). At higher dose, a trend of precipitate dissolution occurring under disordered state was observed, which is due to the ballistic mixing effect by irradiation. However, at temperatures greater than 773 K (500 °C), the precipitates stayed ordered up to 5.4 dpa, supporting the view that irradiation-induced disordering/dissolution and thermal recovery reach a balance between 673 K and 773 K (400 °C and 500 °C). Effects of Ti/Al ratio and irradiation dose rate are also discussed.     

Microstructure,Texture, and Mechanical Properties of <Emphasis Type="Italic">β</Emphasis> Solution-Treated and Aged Metastable <Emphasis Type="Italic">β</Emphasis> Titanium Alloy,Ti-5Al-5Mo-5V-3Cr

The current study describes the aging characteristics and mechanical properties of a metastable β titanium alloy Ti-5Al-5Mo-5V-3Cr. The aged microstructures consist of fine α-phase precipitates (lath morphology) in equiaxed β grains. The sizes of the α-phase precipitates increase with the increasing aging temperature. The β ST WQ and 823 K (550 °C)-aged material exhibits maximum hardness due to precipitation hardening. The low- and high-temperature aging conditions result in strong c-type basal and prismatic textures in the α-phase, respectively. The β-phase of the alloy aged at low temperature reveals the presence of texture with moderate intensity. In contrast, high-temperature-aged material exhibits very strong β-phase texture. The strengths of the alloy under β ST WQ- and 923 K (650 °C)-aged conditions are the maximum and minimum along TD and RD, while the ductility values are the maximum and minimum along the RD and TD direction samples, respectively. The flow curves follow typical Holloman equation along three sample directions, and the work hardening rate curves display two distinctive regimes, namely, stage I and stage II. The yield locus plots of the β ST WQ and aged materials exhibit the presence of anisotropy.     

Design of strong tough Fe/Mo/C martensitic steels and the effects of cobalt

The microstructures and mechanical properties of a series of vacuum melted Fe/(2 to 4) Mo/(0.2 to 0.4) C steels with and without cobalt have been investigated in the as-quenched fully martensitic condition and after quenching and tempering for 1 h at 673 K (400°C) and 873 K (600°C); austenitizing was done at 1473 K (1200°C) in argon. Very good strength and toughness properties were obtained with the Fe/2 Mo/0.4 C alloy in the as-quenched martensitic condition and this is attributed mainly to the absence of internal twinning. The slightly inferior toughness properties compared to Fe/Cr/C steels is attributed to the absence of interlath retained austenite. The two 0.4 pct carbon steels having low Mo contents had approximately one-half the amount of transformation twinning associated with the two 0.4 pct carbon steels having high Mo contents. The plane strain fracture toughness of the steels with less twinning was markedly superior to the toughness of those steels with similar alloy chemistry which had more heavily twinned microstructures. Experiments showed that additions of Co to a given Fe/Mo/C steel raised M_s but did not decrease twinning nor improve toughness. Molybdenum carbide particles were found in all specimens tempered at 673 K (400°C). The Fe/Mo/C system exhibits secondary hardening after tempering at 873 K (600°C). The precipitate is probably Mo₂C. This secondary hardening is associated with a reduction in toughness. Additions of Co to Fe/Mo/C steels inhibited or eliminated the secondary hardening effect normally observed. Toughness, however, did not improve and in fact decreased with Co additions.     

Microstructural Evolutions During Thermal Aging of Alloy 625: Impact of Temperature and Forming Process

The microstructural evolutions occurring upon thermal aging of alloy 625 sheets were studied in the 823 K to 1173 K (550 °C to 900 °C) temperature range and for durations up to 2000 hours. TTT diagrams of the δ and γ″ phases were established based on high-resolution scanning electron microscopy and associated quantitative image analysis approaches. The evolutions of secondary carbide volume fraction were also characterized. It was observed that the precipitation domains of the γ″ and δ phases are, respectively, 823 K to 1023 K (550 °C to 750 °C) and 923 K to 1173 K (650 °C to 900 °C) and that the γ″ coarsening follows the LSW theory once these particles have an ellipsoidal morphology. The onset of grain growth, accompanied with an increase of the texture index, was observed at a temperature as low as 1173 K (900 °C). It results from the progressive dissolution of grain boundaries’ secondary carbides (especially M₆C carbides) at this temperature, a process that favors a greater mobility of grain boundaries. It is also shown that the forming process (shear spinning), even after a relaxation heat treatment, enhances and stabilizes the precipitation of the δ phase compared to as-rolled + solution heat-treated sheets. It hence slows down the precipitation of the γ″ phase, a result that is in good agreement with a thermal aging that was performed under load (i.e., during a creep test).     

Design of strong tough Fe/Mo/C martensitic steels and the effects of cobalt

The microstructures and mechanical properties of a series of vacuum melted Fe/(2 to 4) Mo/(0.2 to 0.4) C steels with and without cobalt have been investigated in the as-quenched fully martensitic condition and after quenching and tempering for 1 h at 673 K (400°C) and 873 K (600°C); austenitizing was done at 1473 K (1200°C) in argon. Very good strength and toughness properties were obtained with the Fe/2 Mo/0.4 C alloy in the as-quenched martensitic condition and this is attributed mainly to the absence of internal twinning. The slightly inferior toughness properties compared to Fe/Cr/C steels is attributed to the absence of interlath retained austenite. The two 0.4 pct carbon steels having low Mo contents had approximately one-half the amount of transformation twinning associated with the two 0.4 pct carbon steels having high Mo contents. The plane strain fracture toughness of the steels with less twinning was markedly superior to the toughness of those steels with similar alloy chemistry which had more heavily twinned microstructures. Experiments showed that additions of Co to a given Fe/Mo/C steel raisedM _S but did not decrease twinning nor improve toughness. Molybdenum carbide particles were found in all specimens tempered at 673 K (400°C). The Fe/Mo/C system exhibits secondary hardening after tempering at 873 K (600°C). The precipitate is probably Mo₂C. This secondary hardening is associated with a reduction in toughness. Additions of Co to Fe/Mo/C steels inhibited or eliminated the secondary hardening effect normally observed. Toughness, however, did not improve and in fact decreased with Co additions.     

Influence of the Processing Temperature on the Microstructure, Texture, and Hardness of the 7075 Aluminum Alloy Fabricated by Accumulative Roll Bonding

The 7075 alloy is an Al-Zn-Mg-Cu wrought age-hardenable aluminum alloy widely used in the aeronautical industry. The alloy was accumulative roll bonded at 300 °C (573 K), 350 °C (623 K), and 400 °C (673 K), and the microstructure, texture, and hardness were investigated. Cell/(sub)grain size in the nanostructured range, typical β-fiber rolling texture, and homogeneous hardness through thickness were determined in all cases. Misorientation was different at each processing temperature. At 400 °C, the presence of elements in solid solution and the partial dissolution of the hardening precipitates lead to a poorly misoriented microstructure with a high dislocation density and a homogeneous β-fiber texture of low intensity, typical of intermediate degrees of rolling. At 350 °C and 300 °C, highly misoriented microstructures with smaller dislocation density and intense heterogeneous β-fiber rolling texture are observed, especially at 350 °C, wherein the degree of dynamic recovery (DRV) is higher. Hardness of the accumulative roll bonded samples is smaller than that of the starting material due to particle coarsening, and it is affected by solid solution and/or by fine precipitates produced by reprecipitation of the elements in solid solution.     

Acceleration or Suppression of α-Phase Precipitation Using Isothermal ω Phase in Ti-20 at.pct Nb Alloy

Homogeneous precipitation of a fine α phase in the β matrix of Ti alloys is a promising method for obtaining a highly strengthened Ti-based alloy. Isothermal ω particles are known to be the nucleation sites for fine α-phase precipitation, but an understanding of the kinetics of α-phase formation on isothermal ω particles is still lacking. This study aimed to reveal the effect of isothermal ω particles on α-phase precipitation onset time. Two-step isothermal aging of a Ti-20 at.pct Nb alloy after solid solution treatment at 1273 K (1000 °C) was carried out. The first step of the aging at 633 K (360 °C) involved the formation of isothermal ω particles in the β matrix. This was followed by a second aging step at 673 K, 723 K, and 773 K (400 °C, 450 °C, and 500 °C) for α-phase precipitation. Suppression of α-phase nucleation on the isothermal ω particles occurred at 673 K (400 °C), whereas acceleration of α-phase nucleation on the isothermal ω particles was observed at 723 K and 773 K (450 °C and 500 °C). Thermodynamic stability of the isothermal ω particles and solute partitioning were controlling factors for the α-phase precipitation kinetics.     

Age Hardening Behavior and Corresponding Microstructure of Dilute Al-Er-Zr Alloys

The age hardening and the microstructure of dilute Al-Er-Zr alloys were investigated by microhardness tests and TEM. The Al-0.04Er alloy shows a conventional age hardening behavior and obtains a maximum hardness of 410 MPa after aging for 2 h at 523 K (250 °C) due to precipitation of Al₃Er. The addition of Zr to Al-Er alloy can slow down the growth of the precipitates and make the age hardening effect remain for a long time in Al-0.04Er-0.04Zr alloy. Addition of Zr retards the decomposition of Al-Er and the Al-0.04Er-0.08Zr alloy can reach higher peak hardness than that of Al-0.04Er after aging for long time at elevated temperature. The precipitation behavior of Al-Er-Zr system is likely to be a new commercial way to developing creep-resistant aluminum alloy.     

748 K (475 °C) Embrittlement of Duplex Stainless Steel: Effect on Microstructure and Fracture Behavior

22Cr-5Ni duplex stainless steel (DSS) was aged at 748 K (475 °C) and the microstructure development correlated to changes in mechanical properties and fracture behavior. Tensile testing of aged microstructures confirmed the occurrence of 748 K (475 °C) embrittlement, which was accompanied by an increase of strength and hardness and loss of toughness. Aging caused spinodal decomposition of the ferrite phase, consisting of Cr-enriched α″ and Fe-rich α′ and the formation of a large number of R-phase precipitates, with sizes between 50 and 400 nm. Fracture surface analyses revealed a gradual change of the fracture mode from ductile to brittle delamination fracture, associated with slip incompatibility between ferrite and austenite. Ferrite became highly brittle after 255 hours of aging, mainly due to the presence of precipitates, while austenite was ductile and accommodated most plastic strain. The fracture mechanism as a function of 748 K (475 °C) embrittlement is discussed in light of microstructure development.     

Aging Degradation of Austenitic Stainless Steel Weld Probed by Electrochemical Method and Impact Toughness Evaluation

The present study discriminates the spinodal decomposition and G-phase precipitation in stainless steel welds by double loop electrochemical potentio-kinetic reactivation method and correlates it with the degradation in toughness property. The welds produced with different heat inputs were aged up to 10,000 hours at 673 K to 723 K (400 to 450 °C) and evaluated subsequently for the degree of sensitization (DOS) and impact toughness. The DOS values obtained were attributed to the spinodal decomposition and precipitation of G-phase. Study shows that the DOS correlates well with the impact toughness of the 304LN weld. Prolonged aging at 673 K and 723 K (400 °C and 450 °C) increased the DOS values while the impact toughness was decreased. The weld fabricated at 1 kJ/mm of heat input, produced higher DOS, compared to that at 3 kJ/mm. The geometrical location along the weld is shown to influence the DOS; higher values were obtained at the root than at the topside of the weld. Vermicular and columnar microstructure, in addition to the spinodal decomposition and G-phase precipitation, observed in the root side of the weld appear risky for the impact toughness.     

Effect of Destabilizing Heat Treatment on Solid-State Phase Transformation in High-Chromium Cast Irons

This work describes the influence of secondary carbide precipitation at destabilizing heat treatment on kinetics of austenite phase transformation at a subcritical range of temperatures in high-Cr cast irons, alloyed with 4 to 6 wt pct of Mn or by complex Mn-Ni-Mo (Mn-Cu-Mo). The samples were soaked at 1073 K to 1373 K (800  °C to 1100  °C) (destabilization) or at 573 K to 973 K (300  °C to 700  °C) (subcritical treatment); the combination of destabilization and subcritical treatment was also used. The investigation was carried out with application of optical and electron microscopy and bulk hardness measurement. Time-temperature-transformation (TTT) curves of secondary carbide precipitation and pearlite transformation for as-cast austenite and destabilized austenite were built in this work. It was determined that the secondary carbide precipitation significantly inhibited the pearlite transformation rate at 823 K to 973 K (550  °C to 700  °C). The inhibition effect is more evident in cast irons alloyed with complex Mn-Ni-Mo or Mn-Cu-Mo. The possible reasons for transformation decelerating could be austenite chemical composition change (enriching by Ni, Si, and Cu, and depleting by Cr) and stresses induced by secondary carbide precipitation.     

Transformation squence in a Cu-Al-Ni shape memory alloy at elevated temperatures

Precipitation sequences in a Cu-14 pct Al-4 pct Ni (wt pct) shape memory alloy were studied by means of transmission electron diffraction and microscopy as well as X-ray microanalysis techniques. On aging thin foil specimens up to 550 °C in the electron microscope, an as-quenched sample having a mixture of 2H-type and D0₃-type metastable structures transformed to the stable simple cubic γ₂ phase at or above 450 °C. The remaining matrix either showed precipitates of the fcc α-phase on prolonged annealing at 500 to 550 °C for a longer period, or transformed to martensite on cooling below theM _s temperature (~150 °C).     

Negative Strain-Rate Sensitivity of Mg Alloys Containing 18R and 14H Long-Period Stacking-Ordered Phases at Intermediate Temperatures

The strain-rate sensitivity of a Mg-10Dy-1Zn (wt pct) alloy containing different long-period stacking-ordered (LPSO) phases has been investigated in the strain rate range of 10^?3 to 1 s^?1 from room temperature to 673 K (400 °C). Both alloys containing 18R-LPSO and 14H-LPSO phases show negative strain-rate sensitivity (–0.02  to –0.01) at intermediate temperatures [423 K to 523 K (150 °C to 250 °C)]. The serration behavior of the Mg-10Dy-1Zn alloy containing 18R-LPSO phase is related to dynamic strain aging. However, the appearance of serrated flow in the Mg-10Dy-1Zn alloy containing 14H-LPSO phase is mostly rooted in the formation of microcracks in \( \left\{ {10\overline{1} 2} \right\} \) planes.     

Precipitates and Grain Boundary Strength of an Fe-Mn-Ni Alloy

The effect of grain boundary (GB) precipitates on the GB strength of an age-hardened Fe-7.8Mn-8.2Ni alloy was investigated. Premature intergranular fracture was observed after age hardening due to the precipitation of ??-MnNi precipitates at prior austenite grain boundaries. However, the conversion of GB ?? precipitates to austenite by a short second aging at 793?K (520?°C) after peak aging at 713?K (440?°C) resulted in a remarkable improvement of GB strength. The result strongly supports the proposition that the weak bonding of GB ?? precipitates to the matrix is the main reason for GB embrittlement in age-hardened Fe-Mn-Ni alloys.     

Decomposition of Fe-Ni martensite: Implications for the low-temperature (≤500 °C) Fe-Ni phase diagram

The low-temperature (<500 °C) decomposition of Fe-Ni martensite was studied by aging martensitic Fe-Ni alloys at temperatures between 300 °C and 450 °C and by measuring the composition of the matrix and precipitate phases using the analytical electron microscope (AEM). For aging treatments between 300 °C and 450 °C, lath martensite in 15 and 25 wt pct Ni alloys decomposed with γ [face-centered cubic (fcc)] precipitates forming intergranularly, and plate martensite in 30 wt pct Ni alloys decomposed with γ (fcc) precipitates forming intragranularly. The habit plane for the intragranular precipitates is {111}_fcc parallel to one of the {110}_bcc planes in the martensite. The compositions of the γ intergranular and intragranular precipitates lie between 48 and 58 wt pct Ni and generally increase in Ni content with decreasing aging temperature. Diffusion gradients are observed in the matrix α [body-centered cubic (bcc)] with decreasing Ni contents close to the martensite grain boundaries and matrix/precipitate boundaries. The Ni composition of the matrix α phase in decomposed martensite is significantly higher than the equilibrium value of 4 to 5 wt pct Ni, suggesting that precipitate growth in Fe-Ni martensite is partially interface reaction controlled at low temperatures (<500 °C). The results of the experimental studies modify the γ/α + γ phase boundary in the present low-temperature Fe-Ni phase diagram and establish the eutectoid reaction in the temperature range between 400 °C and 450 °C. Formerly Research Assistant, Department of Materials Science and Engineering, Lehigh University     

Effects of the Process Parameters on the Microstructure and Properties of Nitrided 17-4PH Stainless Steel

The effects of process parameters on the microstructure, microhardness, and dry-sliding wear behavior of plasma nitrided 17-4PH stainless steel were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and wear testing. The results show that a wear-resistant nitrided layer was formed on the surface of direct current plasma nitrided 17-4PH martensitic stainless steel. The microstructure and thickness of the nitrided layer is dependent on the treatment temperature rather than process pressure. XRD indicated that a single α _N phase was formed during nitriding at 623 K (350 °C). When the temperature increased, the α _N phase disappeared and CrN transformed in the nitrided layer. The hardness measurement demonstrated that the hardness of the stainless substrate steel increased from 320 HV_0.1 in the untreated condition increasing to about 1275HV_0.1 after nitriding 623 K (350 °C)/600 pa/4 hours. The extremely high values of the microhardness achieved by the great misfit-induced stress fields associated with the plenty of dislocation group and stacking fault. Dry-sliding wear resistance was improved by DC plasma nitriding. The best wear-resistance performance of a nitrided sample was obtained after nitriding at 673 K (350 °C), when the single α _N-phase was produced and there were no CrN precipitates in the nitrided layer.