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The liquidus surface projection and isothermal section at 1,800°C in the Mo–Ti–C ternary system are examined using arc-melted alloys. A ternary transition peritectic reaction (L + Mo2C → Mo + TiC) takes place during solidification, which is apparently different from the ternary eutectic reaction (L → Mo + TiC + Mo2C) observed in a previous report. Since the composition of the eutectic reaction (L → Mo + TiC) shifts toward the Mo–Ti binary line with increasing Ti concentration, the volume fraction of the Mo phase and the interlamellar spacing of the Mo and TiC phases increase in the eutectic microstructure. At 1,800°C, the TiC phase in equilibrium with the Mo phase can contain more than 28 at% Mo and a Mo/TiC/Mo2C three-phase region exists at around Mo–15Ti–10C.

A novel procedure of ODS alloy fabrication was examined using a model alloy in the Fe Al O ternary system. Nano-sized Al oxides were precipitated within the α-Fe matrix through a reaction between Fe Al and Fe2O3 powders. Two types of oxides, FeAl2O4 and γ-Al2O3, were found to precipitate during sintering at 1000 °C and the subsequent annealing at 800 °C. The oxides showed sluggish coarsening at 800 °C, which then provided high resistance to coarsening for the α-Fe grains. Microstructure observation and Vickers hardness measurement indicated that the homogeneous dispersion of oxides was achieved through the present procedure without ball milling.

The relation of creep rupture life to minimum creep rate, namely Monkman-Grant (MG) relation is examined by using a creep database of modified 9Cr-1Mo steel. The database covers wide ranges of creep rupture life up to 1.2 × 105 h and of minimum creep rate down to 7.6 × 10−8 h−1. The MG plot exhibits a low overall value of MG exponent (p = 0.85) together with wide scatter of data points at long rupture life. Causes of the low p value and the wide scatter are discussed in the present study paying attention to change in creep curve shape with creep rupture life. There are four regions H, M, L1 and L2 showing different creep behavior in the steel. Regional MG relations are examined also in each region. Values of p are less than unity and change among the four regions. The p value is especially low (0.62) in long-term region L2. The regional p values less than unity result in the low overall p value of 0.85. The especially low regional value of p in the long-term region causes the wide scatter of data points in the overall MG plot. A modified Monkman-Grant equation (Eq. (29)) is proposed taking account of creep deceleration rate A (=−1/(dln e ˙ /de), where e ˙ and e are the creep strain rate and the creep strain) in primary creep and creep acceleration rate B (=1/(dln e ˙ /de)) in tertiary creep. The rates characterize shape of a creep curve. The modified equation can explain the difference of p values among the four regions.

Grade 91 steel is widely used as steam pipes in ultrasupercritical (USC) steam boilers. In residual creep life assessment of the pipes by calculation, one needs creep rupture life of the steel as a function of stress and temperature in a time range longer than 105 h. Four regions with different creep rupture characteristics appear in a stress versus creep rupture life diagram of the steel. Main steam pipes made of the steel are used in a long-term region with low values of stress exponent and activation energy for creep rupture life (referred to as region G in this paper). Creep rupture lives of the steel in this region vary from heat to heat depending on their prior austenite grain size. This paper proposes a grain size-dependent equation representing creep rupture life of the steel in region G. The equation is verified with creep rupture data up to 232,833 h at 600 °C. Region G is absent in some heats with a large grain size. The equation can rationalize the absence in the heats. In a stress versus creep rupture life diagram of grade 92 steel, there is the same long-term region G. In the region, a creep rupture life of each heat is dependent on its grain size as is the case in grade 91 steel. The proposed equation accords well with the creep rupture lives of the grade 92 steel in region G.

In this study, the ultrahigh-temperature tensile creep behaviour of a TiC-reinforced Mo-Si-B-based alloy was investigated in the temperature range of 1400–1600 °C at constant true stress. The tests were performed in a stress range of 100–300 MPa for 400 h under vacuum, and creep rupture data were rationalized with Larson-Miller and Monkman-Grant plots. Interestingly, the MoSiBTiC alloy displayed excellent creep strength with relatively reasonable creep parameters in the ultrahigh-temperature range: a rupture time of ~400 h at 1400 °C under 137 MPa with a stress exponent (n) of 3 and an apparent activation energy of creep (Qapp) of 550 kJ/mol. The increasing rupture strains with decreasing stresses (up to 70%) and moderate strain-rate oscillations in the creep curves suggest that two mechanisms contribute to the creep: phase boundary sliding between the hard T2 and (Ti,Mo)C phases and the Moss phase, and dynamic recovery and recrystallization in Moss, observed with orientation imaging scanning electron microscopy. The results presented here represent the first full analysis of creep for the MoSiBTiC alloy in an ultrahigh-temperature range. They indicate that the high-temperature mechanical properties of this material under vacuum are promising.

Larson-Miller (LM) and Orr-Sherby-Dorn (OSD) parameters are widely used when formulating and predicting creep rupture life tr. The LM constant C and the activation energy Q in the OSD parameter characterize temperature dependence of tr. Q = QLSD (QLSD: activation energy for lattice self-diffusion) and C = 20 are often assumed in the formulation. Creep rupture datasets of 11 heats of nickel alloy A617, 304H and 304J1 stainless steels, 6 heats of A3004N aluminum alloy and four Mg-Al alloys are formulated with the parameters for determining C and Q of each dataset. Based on the correlation between C and Q among similar materials, it is discussed what is the C value equivalent to Q = QLSD. It is also examined how the C value changes with melting temperature of the material. The value of C equivalent to Q = QLSD varies from 14 to 9.5 depending on average values of log(rupture life) and of reciprocal temperature of the dataset. These values of C point out that C = 20 is not equivalent to Q = QLSD. The equivalent C values are similar in all the materials independently of their melting temperatures.

The liquidus projection and the invariant reactions associated with the liquid phase in the Zr-Si-Al ternary system were experimentally determined. Seventeen primary phase regions were identified from metallographic observation and analysis of the as-cast microstructures. There are at least sixteen invariant reactions and three local maxima associated with congruent melting in the ternary system. The ZrSi primary solidification region covers a wide range of compositions in the Zr-Si-Al ternary system. A variety of the solidification paths were described.

Boron segregation behavior during tempering at 600 and 790 °C was examined in a boron-doped 9Cr-steel by using high-resolution SIMS imaging (nano-SIMS). Boron segregation that developed at prior austenite grain boundaries (PAGBs) during austenitizing was found to decrease reduced during tempering because the equilibrium concentration of B segregation for austenite is larger than that for ferrite so that the segregated boron atoms diffused into block and packet boundaries. The size and the volume fraction of the carbide precipitates at PAGBs were smaller than those at packet boundaries, suggesting that boron segregation at PAGBs suppresses the carbide precipitation upon tempering.

YB4/YB6 two-phase alloys were prepared by arc-melting of high purity elemental materials. The Young's moduli of YB4 and YB6 were evaluated by nanoindentation technique. During loading of nanoindentation, pop-in events were clearly observed for YB4 and YB6, suggesting that both have some capability of dislocation emission at room temperature. TEM observation depicts that dislocations have formed in YB4 and YB6 due to the thermal stress that developed during cooling following arc-melting. The Burgers vectors of these dislocations were identified to be [001] for YB4, and 〈100〉 for YB6. Potential slip systems that are indicated to operate were (100)[001] for YB4 and {100}〈001〉 for YB6.

Heat-to-heat variation of creep strength is significant in grade 91 (Gr.91) steel, but the causes of the variation have not been well understood yet. In the present paper, creep rupture data of 14 heats of Gr.91 steel were analyzed paying attention to their chemical compositions and microstructures. The longest creep rupture lives analyzed are 2 × 105 h at 500 and 550 °C and 105 h at 600 °C. The causes of the heat-to-heat variation are different, depending on creep test conditions. At low temperature and high stress (creep rupture life of 104 h at 500 and 550 °C), creep rupture strength increases with increase of hardness after tempering. This suggests strengthening by a fine subgrain microstructure developed during normalizing and subsequent tempering. At higher temperature and intermediate time range (104 h at 600 °C), creep rupture strength depends on Cr concentration of the heats in addition to the hardness. This finding suggests an important contribution of recovery process of the subgrain microstructures to creep strength of the steel. In long-term creep (2×105 h at 550 °C and 105 h at 600 °C) creep rupture strength primarily increases with increasing grain size of the heats. This suggests that grain boundary sliding is an important deformation mode at low strain rate because of fine grain size usual with Gr.91 steel. Specifications on Ni concentration and N%/Al% ratio are newly introduced in the type II version of Gr.91 steel. They are not effective to eliminate a heat with low creep strength.

Al3Nb is known as a high oxidation resistant material, while it is quite brittle. As the fracture toughness of Al3Nb single crystal and its dependence on the composition are not obtained, the micro-sized fracture testing proposed by Suzuki et al. was performed. Al3Nb single crystal micron-order size cantilevers with a chevron-notch were fabricated in a grain of two-phase polycrystalline alloys by using FIB (Focused Ion Beam). From the load-displacement curves during the bending by a nanoindenter, the average value of fracture toughness of Nb-rich Al3Nb is evaluated to be 2.90 MPam1/2, while the fracture toughness of Al-rich Al3Nb is also evaluated to be 2.82 MPam1/2. From this result, the fracture toughness of Al3Nb is less dependent on its Al/Nb ratio. Furthermore the fracture toughness of Al3 (Nb, V) was evaluated to be 2.82 MPam1/2.The fracture toughness of Al3Nb is seemingly insensitive to V addition.

The applicability of radio frequency glow discharge (rf-GD) sputtering to the surface finishing of nanoindentation specimens was examined for pure Al, Cu, and Ni. Comparisons were made between specimens that had been subjected to the following surface finishing: (1) rf-GD sputtering, (2) electropolishing, and (3) mechanical polishing with 0.25 µm of diamond suspension. It was suggested from the nanoindentation behavior and the quality of electron backscattered diffraction patterns that residual damage on the surface of the rf-GD sputtered samples was as small as that of electropolished samples, while some damages remained on the surface of the mechanically polished samples. The areal roughness within a 1-μm square of the rf-GD sputtered surface was comparable to that of the mechanically polished surface and slightly larger than that of the electropolished surface. Nonetheless, the difference of the roughness within the range of this study has no practical impact upon nanohardness and elastic modulus evaluation. Pop-in events occurred in the electropolished and rf-GD sputtered specimens, but not in the mechanically polished samples. The critical load for pop-in to occur was slightly smaller in rf-GD sputtered sample than in electropolished samples.

The present paper studies stress, temperature and heat dependence of creep rupture life of 9Cr-1.8W-0.5Mo-VNb (Gr. 92) steel with creep rupture data of 4 heats reported in National Institute for Materials Science Creep Data Sheet 48B. In creep of Gr. 92 steel there are four regions, H, M, L and G, showing different stress and temperature dependence of creep rupture life. Creep rupture life of Gr. 92 steel increases with increasing hardness after tempering in Regions H and M (high and medium stress), and with increasing prior austenite grain size in long-term Region G. Its creep rupture life is insensitive to the heats in low-stress Region L. Creep rupture lives of the steel are formulated in each region as a function of stress, temperature and a metallurgical variable determining its creep rupture life. Two types of breakdown in creep strength (substantial decrease in stress exponent for creep rupture life) take place in Gr. 92 steel; one from Region M to Region L, and the other from Region M or L to Region G. Since Gr. 92 steel is used in Region G in steam power boilers, the second breakdown to Region G is of engineering importance. Causes of the second breakdown are discussed with creep rupture data of four grades of creep strength enhanced ferritic steels.

The three-phase, (Mo,Nb) ss /(Mo,Nb) 5 Si 3 /(Mo,Nb) 5 SiB 2 , Bcc/T 1 /T 2 microstructures that develop in Mo–Nb–Si–B alloys have been examined in arc cast and directionally solidified samples to identify the phase sequencing during solidification. A Mo-32.6Nb-19.5Si-4.7B (at.%) alloy was directionally solidified using an optical floating zone (OFZ) furnace in a flowing Ar gas atmosphere at a constant growth rate of 10 mm/h. The microstructure of the directionally solidified alloy is characterized by an elongated T 2 phase surrounded by bcc and T 1 phases with an interwoven morphology From the evaluation of the microstructures in arc cast ingots of several alloys at a constant 32.6 at%Nb composition, the path of the liquidus valleys with decreasing temperature has been determined to intersect at a common point that establishes the solidification reaction as a eutectic. The incorporation of the experimental results into a computational thermodynamic analysis provides insight on the partitioning of components within each phase during solidification.

The effects of the Ti content on the microstructure and oxidation behaviour of Mo–yTi–14Si–6C–6B (atom %) alloys were investigated. Enrichment with Ti of up to 54% did not change the four-phase constitution of the Moss, Mo5SiB2, Ti5Si3, or TiC phase, and improved the oxidation resistance of the alloy. The Mo–50Ti–14Si–6C–6B alloy exhibited the best oxidation resistance at 800–1200 °C through formation of a dense layer of TiO2. This improvement can be described in terms of a modified Pilling–Bedworth ratio, which indicated that the densest TiO2 layer formed on Moss grains.

The oxidation behavior of a Ti5Si3-incorporated MoSiBTiC alloy (38Mo–30Ti–17Si–10C–5B, at.%) was systematically studied in the temperature range of 700–1000 °C. Temperature dependence of oxidation kinetics and oxide scale formation was revealed for this alloy. The oxidation kinetics at 700 °C featured an initial transient stage of weight gain and then switched to weight loss. At 800 °C, the oxidation kinetics featured an initial transient stage with fast weight loss, a steady stage with small weight loss, and an acceleration stage leading to catastrophic failure. At 900 and 1000 °C, the alloy exhibited a rapid transient weight loss as followed by a decreased weight loss fitting to parabolic kinetics. The scales that formed at 700–1000 °C mainly consisted of rutile TiO2 and amorphous SiO2. The high viscosity of SiO2 at 700 and 800 °C caused the formation of porous and microcracked oxide scales while the occurrence of viscous flow during oxidation at 900–1000 °C promoted the formation of dense and protective scales.

In this study, the crystallographic orientation relationship between bcc precipitates and a Ti5Si3 matrix in Mo–50Ti–14Si–6C–6B (at.%) alloy was established. The alloy microstructure consisted of the bcc solid solution, Ti5Si3, Mo5SiB2, and TiC phases. The metal-rich Ti5Si3 phase was formed during a solidification stage, followed by the precipitation of the bcc phase within the Ti5Si3 matrix in the subsequent annealing process. The orientation relationship between the two phases was described by the expression: 112 bcc / / 01 1 ‾ 0 Ti 5 Si 3 and 3 ‾ 11 bcc / / 0001 Ti 5 Si 3 . The formation of a low-energy interface between the two phases was explained by the edge-to-edge matching of their corresponding lattice planes at the faceted interface.

The effect of Cr addition on the oxidation behaviour of multiphase Mo–28Ti–14Si–6C–6B (at. %) alloy composed of Mo solid solution, Mo5SiB2, Ti5Si3, and TiC phases was investigated. Replacement of 10 at. % Cr for Mo hardly changed the microstructure of the alloy and significantly enhanced its oxidation resistance at 800 °C. At 1100 °C, the Cr-added MoSiBTiC alloy showed less weight loss than the Cr-free base alloy. However, Cr addition had little effect on the substrate reduction, particularly for longer oxidation periods, due to the high volatility of Cr oxide at higher temperatures.

Predictions as to 105 hrs creep rupture strength of grade 91 steel have been made recently. The predictions should be verified by some means, since they are based on certain assumptions. A formula for predicting long-term creep rupture lives should correctly describe long-term data points used in its formulation. Otherwise the formula cannot properly predict further longer-term creep rupture lives. On the basis of this consideration, the predictions are examined with long-term creep rupture data of the steel. In the predictions three creep rupture databases were used: data of tube products of grade 91 steel reported in NIMS Creep Data Sheet (NIMS T91 database), data of T91 steel collected in Japan, and data of grade 91 steel collected by an ASME code committee. Short-term creep rupture data points were discarded by the following criteria for minimizing overestimation of the strength: selecting long-term data points with low activation energy (multi-region analysis), selecting data points crept at stresses lower than a half of proof stress (σ0.2/2 criterion), and selecting data points longer than 1000 hrs (cut-off time of 1000 hrs). In the case of NIMS T91 database, a time-temperature parameter (TTP) analysis of a dataset selected by the multi-region analysis can properly describe the long-term data points. However, the TTP analyses of datasets selected by the σ0.2/2 criterion and by the cut-off time of 1000 hrs from the same database overestimate the long-term data points. The different criteria for data selection have more substantial effects on predicted values of the strength of the steel than difference of the databases.

We systematically investigate stress–strain behavior of ferrite and bainite with nano-sized vanadium carbides in low carbon steels; the ferrite samples were obtained through austenite/ferrite transformation accompanied with interphase precipitation and the bainite samples were via austenite/bainite transformation with subsequent aging. The stress–strain curves of both samples share several common features, i.e. high yield stress, relatively low work hardening and sufficient tensile elongation. Strengthening contributions from solute atoms, grain boundaries, dislocations and precipitates are calculated based on the structural parameters, and the calculation result is compared with the experimentally-obtained yield stress. The contributions from solute atoms and grain boundaries are simply additive, whereas those from dislocations and precipitates should be treated by taking the square root of the sum of the squares of two values. Nano-sized carbides may act as sites for dislocation multiplication in the early stage of deformation, while they may enhance dislocation annihilation in the later stage of deformation. Such enhanced dynamic recovery might be the reason for a relatively large elongation in both ferrite and bainite samples.

Predictions as to 105 h creep rupture strength of grade 91 steel have been made recently. The predicted values are examined with long-term creep rupture data of the steel. Three creep rupture databases were used in the predictions: data of tube products of grade 91 steel reported in National Institute for Materials Science (NIMS) Creep Data Sheet (NIMS T91 database), data of T91 steel collected in Japan, and data of grade 91 steel collected by an American Society of Mechanical Engineers (ASME) code committee. Short-term creep rupture data points were discarded by the following criteria for minimizing overestimation of the strength: selecting long-term data points with low activation energy (multiregion analysis), selecting data points crept at stresses lower than a half of proof stress (σ0.2/2 criterion), and selecting data points longer than 1000 h (cutoff time of 1000 h). In the case of NIMS T91 database, a time–temperature parameter (TTP) analysis of a dataset selected by multiregion analysis can properly describe the long-term data points and gives the creep rupture strength of 68 MPa at 600 °C. However, TTP analyses of datasets selected by σ0.2/2 criterion and cutoff time of 1000 h from the same database overestimate the data points and predict the strength over 80 MPa. Datasets selected by the same criterion from the three databases provide similar values of the strength. The different criteria for data selection have more substantial effects on predicted values of the strength of the steel than difference of the databases.

The phase equilibrium and oxidation behavior of the disilicides that form in the Nb-Cr-Si ternary system have been investigated. Although NbSi2 and CrSi2 both exhibit a C40 crystal structure, they form separate ranges of compositional homogeneity in the ternary system. Their phase boundaries at 1300 °C have been experimentally determined in this study. The binary NbSi2 exhibited poor oxidation resistance, showing pest-like behavior during oxidation at temperature above 800 °C. In contrast, the alloys containing Cr showed much better oxidation resistance up to 1200 °C.

A micro-sized fracture testing method has been applied to investigate fracture toughness of alpha-Nb5Si3. Chevron-notched single crystal specimens with a size of 3 x 3 x 15 μm3 were prepared in a grain of polycrystalline alpha-Nb5Si3 by focused ion beam, FIB, technique. Fracture tests were conducted using a nanoindenter at room temperature and linear load-displacement curves and smooth fracture surfaces were obtained. This fracture behavior was presumed to be brittle fracture similar to bulk alpha-Nb5Si3. The average of fracture toughness KQ is 3.45 ± 0.29 MPa√m under a small-scale yielding condition.