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

Effect of carbon concentration on precipitation behavior of M<Subscript>23</Subscript>C<Subscript>6</Subscript> carbides and MX carbonitrides in martensitic 9Cr steel during heat treatment

The distributions and precipitated amounts of M₂₃C₆ carbides and MX-type carbonitrides with decreasing carbon content from 0.16 to 0.002 mass pct in 9Cr-3W steel, which is used as a heat-resistant steel, has been investigated. The microstructures of the steels are observed to be martensite. Distributions of precipitates differ greatly among the steels depending on carbon concentration. In the steels containing carbon at levels above 0.05 pct, M₂₃C₆ carbides precipitate along boundaries and fine MX carbonitrides precipitate mainly in the matrix after tempering. In 0.002 pct C steel, there are no M₂₃C₆ carbide precipitates, and instead, fine MX with sizes of 2 to 20 nm precipitate densely along boundaries. In 0.02 pct C steel, a small amount of M₂₃C₆ carbides precipitate, but the sizes are quite large and the main precipitates along boundaries are MX, as with 0.002 pct C steel. A combination of the removal of any carbide whose size is much larger than that of MX-type nitrides, and the fine distributions of MX-type nitrides along boundaries, is significantly effective for the stabilization of a variety of boundaries in the martensitic 9Cr steel.     

Reduction kinetics of Fe<Subscript>2</Subscript>MoO<Subscript>4</Subscript> fine powder by hydrogen in a fluidized bed

Iron molybdate (Fe₂MoO₄) powders with an average particle size of 100 μm were reduced by hydrogen using a fluidized-bed batch reactor in the temperature range of 923 to 1173 K. The extent of the reaction was followed as a function of time by gas chromatography. The fluidizing-gas velocity was set at about 1.5 times the minimum fluidization velocity. The ratio of the height of the static bed to its diameter is about 1. Under the prevailing experimental conditions, it was found that the chemical reaction was the rate-controlling factor. The activation energy for this process was 158±17 kJ/mol. The crystal size of the Fe₂Mo powder produced at lower temperatures was in the nanometer range, indicating the possibility of mass production of alloys and intermetallics in the nanorange, using a fluidized bed.     

Reduction of Fe<Subscript>2</Subscript>MoO<Subscript>4</Subscript> by hydrogen gas

In the present work, the reduction kinetics of iron molybdate (Fe₂MoO₄) by hydrogen gas was investigated by thermogravimetric analyses (TGA). Both isothermal and nonisothermal experiments were conducted. By using fine particles, very shallow powder bed, and high hydrogen flow rate, the study could be focused on the chemical reaction. The activation energy obtained from the isothermal experiments was found to be 173.5 kJ/mol, which was in reasonable agreement with the value of 158.3 kJ/mol obtained from the nonisothermal experiments. The reduction product was found to be an intermetallic compound, Fe₂Mo, of microcrystalline structure.     

Effect of Planar Flow Melt Spinning Parameters on Ribbon Formation in Soft Magnetic Fe<Subscript>68.5</Subscript>Si<Subscript>18.5</Subscript>B<Subscript>9</Subscript>Nb<Subscript>3</Subscript>Cu<Subscript>1</Subscript> Alloy

The effect of planar flow melt spinning (PFMS) parameters on the continuity, surface quality, and structure of 10-mm-wide Fe_68.5Si_18.5B₉Nb₃Cu₁ ribbons has been investigated. The change in shape and stability of the melt puddle as a function of the processing parameter was studied using a high-speed imaging system and was correlated to ribbon formation. A window of process parameters for obtaining continuous ribbons with good surface quality has been evaluated. It has been observed that thinner ribbons are found to be more continuous because of higher ductility. The higher melt temperature leads to the formation of crystalline phase in as-spun ribbons, and this deteriorates the soft magnetic properties on annealing. The experimental results are corroborated with the numerical estimates, which suggest that the critical thickness for amorphous phase formation decreases with increasing initial melt temperature.     

Effect of the liquid phase on the formation of orthorhombic boride during the crystallization of Fe<Subscript>82</Subscript>B<Subscript>18</Subscript> amorphous ribbons

Amorphous Fe₈₂B₁₈ ribbons prepared by melt quenching from different temperatures have been studied during step-by-step heating. Depending on the quenching temperature, the crystallization of the ribbons was shown to occur via different mechanisms, namely, with and without the formation of the orthorhombic Fe₃B^orth boride. This is related to different structural states of the melt used for the preparation of the rapidly quenched ribbons. The appearance of the orthorhombic Fe₃B^orth boride is preceded by the crystallization of the amorphous component with the formation of the Fe₃B^tet boride having a distorted body-centered tetragonal lattice.     

Influence of heat treatment on the efficiency of impact fragmentation of amorphous alloy Fe<Subscript>73.5</Subscript>Cu<Subscript>1</Subscript>Nb<Subscript>3</Subscript>Si<Subscript>13.5</Subscript>B<Subscript>9</Subscript> ribbons

The mechanism of impact fracture of soft magnetic amorphous alloy Fe_73.5Cu₁Nb₃Si_13.5B₉ ribbons in a disintegrator after heat treatment at a temperature from the range 300–700°C and the fractional composition of the formed powder are studied. The temperature ranges of a change in the mechanism of ribbon fracture are determined. The particle size distribution is shown to change weakly within the revealed temperature ranges.     

Structure and magnetic properties of the Nd<Subscript>9.5</Subscript>Fe<Subscript>84.5</Subscript>B<Subscript>6</Subscript> alloy subjected to severe plastic deformation and annealing

The effect of severe plastic deformation (SPD) by torsion and subsequent annealing on the structure and magnetic properties of the cast Nd_9.5Fe_84.5B₆ alloy is studied. SPD by torsion is shown to lead to partial amorphization of the Nd₂Fe¹⁴B phase and the precipitation of α-Fe; subsequent annealing results in the crystallization of the amorphous phase and the formation of a nanocomposite Nd₂Fe₁₄B/α-Fe structure. After SPD by torsion at 20 revolutions and annealing at 873 K, the (101) texture is formed; in this case, the coercive force is H _c = 360 kA/m and the maximum energy product is (BH) _max = 166 kJ/m3. The residual magnetization and the squareness ratio of the hysteretic loop of the textured alloy decrease as the ambient temperature decreases.     

The role of microstructural instability on creep behavior of a martensitic 9Cr-2W steel

The microstructural instability during creep and its effect on creep behavior were investigated for a martensitic 9Cr-2W steel. The steel was developed as a low radioactive steel suitable for fusion reactor structure. Creep testing was carried out at 873 K for up to 15,100 ks (4200 hours). The creep curve consisted of transition creep, where creep rate decreased with time, and acceleration creep, where creep rate increased with time. During creep, microstructural instability, such as the recovery of dislocations, the agglomeration of carbides, and the growth of martensite lath subgrains, was observed to occur, which resulted in softening but no hardening. The transition creep was a consequence of the movement and annihilation of excess dislocations, resulting in the decrease in dislocation density and the increase in martensite lath size with time. The acceleration creep was a consequence of a gradual loss of creep strength due to the microstructural instability which occurred from the initial stage of creep.     

Effect of Firing Temperature and Reducing Gas Composition during Low-Temperature Reduction of Nanocrystalline Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>

Pure nanocrystalline hematite (40 to 100 nm) compacts were prepared and sintered at various temperatures (300 °C to 600 °C) and then reduced with 100 pct H₂ at 500 °C. On the other hand, fired compacts at 500 °C were reduced with a H₂-Ar gas mixture containing different concentration of hydrogen (100, 75, 50, and 25 pct) at 500 °C using thermogravimetric techniques. Nanocrystalline Fe₂O₃ compacts were characterized before and after reduction with X-ray diffraction, scanning electron microscopy (SEM), vibrating sample magnetometer (VSM), and reflected light microscope. It was found that the fired compacts at 400 °C to 600 °C have relatively faster reaction behaviors compared to that at lower firing temperature 300 °C. By decreasing the firing temperature to 300 °C, partial sintering with grain growth was observed clearly during reduction. Also, it was found that the reduction rate increased with increasing hydrogen content in the reducing gas. Comparatively, grain growth and partial coalescence took place during reduction with 25 pct H₂ due to long reaction time.

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Effect of Ce<Subscript>2</Subscript>O<Subscript>3</Subscript> on Structure,Viscosity, and Crystalline Phase of CaO-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-Li<Subscript>2</Subscript>O-Ce<Subscript>2</Subscript>O<Subscript>3</Subscript> Slags

Aiming at devising new mold flux for Ce-bearing stainless steel, a fundamental investigation on the effect of Ce₂O₃ on properties of the CaO-Al₂O₃-Li₂O-Ce₂O₃ slag was provided by the present work. The results show that adding Ce₂O₃ could decrease the viscosity of the slag due to its effects on decreasing the polymerization of the slag. The crystalline process was restrained by increasing the content of Ce₂O₃, and the crystalline phases also can be influenced by the slag structure. The crystalline phases were transferred from LiAlO₂ and CaO to LiAlO₂ and CaCeAlO₄ with the addition of Ce₂O₃ to the slag, which could be well confirmed by the structure of the unit cell of the crystals.     

A reinvestigation of phase equilibria in the system Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript>-ZnO

The phase equilibria and liquidus temperatures in the binary SiO₂-ZnO system and in the ternary Al₂O₃-SiO₂-ZnO system at low Al₂O₃ concentrations have been experimentally determined using the equilibration and quenching technique followed by electron probe X-ray microanalysis. In the SiO₂-ZnO system, two binary eutectics involving the congruently melting willemite (Zn₂SiO₄) were found at 1448±5 °C and 0.52±0.01 mole fraction ZnO and at 1502±5 °C and 0.71±0.01 mole fraction ZnO, respectively. The two ternary eutectics involving willemite previously reported in the Al₂O₃-SiO₂-ZnO system were found to be at 1315±5 °C and 1425±25 °C, respectively. The compositions of the eutectics are 0.07, 0.52, and 0.41 and 0.05, 0.28, and 0.67 mole fraction Al₂O₃, SiO₂, and ZnO, respectively. The results of the present investigation are significantly different from the results of previous studies.     

Formation of CaS on Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-CaO inclusions during solidification of steels

In this article, the effect of CaS formation on the evolution of Al₂O₃-CaO inclusions in low-carbon Al-killed and Ca-treated steel during the solidification process is investigated through high-temperature confocal scanning laser microscopy (CSLM). The inclusions started as mostly liquid-globular inclusions that did not agglomerate with each other on the melt surface but during solidification were seen to change shape into an irregular morphology. The shape change was found to be due to the reaction between the Al₂O₃-CaO inclusions with the dissolved S and Al in the melt, resulting in the formation of dense CaS shells around the inclusions. The melt composition during solidification, estimated from the observed solid δ-front advance rate, was compared to the thermodynamic limit for CaS precipitation. The observed growth rate of the CaS shell was found to initially increase with decreasing temperature because of the higher, solid δ-front advance rates at lower temperatures, which results in higher rates of S and Al partitioning. Once CaS had precipitated, the inclusions were found to form agglomerates on the melt surface because of fluid flow, initially, and later, the capillary depression.     

Electrochemical Behavior of an Amorphous and Nanocrystalline Fe<Subscript>79</Subscript>P<Subscript>13</Subscript>Si<Subscript>5</Subscript>V<Subscript>3</Subscript> Alloy in a Damp SO<Subscript>2</Subscript>-Contaminated Atmosphere

The electrochemical behavior of amorphous and nanocrystalline soft magnetic Fe₇₉P₁₃Si₅V₃ alloy in a 0.1 M Na₂SO₄ solution has been studied. Mössbauer studies show that the electrochemical characteristics of the alloy are comparable with those of an Finemet Fe₇₇Si₁₃B₇Nb_2.1Cu_0.9 alloy, whereas the studied alloy is inexpensive and can be prepared using natural alloy ferrophosphorus containing vanadium and silicon.     

Corrosion Behavior of Fe<Subscript>41</Subscript>Co<Subscript>7</Subscript>Cr<Subscript>15</Subscript>Mo<Subscript>14</Subscript>C<Subscript>15</Subscript>B<Subscript>6</Subscript>Y<Subscript>2</Subscript> Bulk Metallic Glass in Sulfuric Acid Solutions

An Fe₄₁Co₇Cr₁₅Mo₁₄C₁₅B₆Y₂ bulk metallic glass with a diameter of 5 mm was prepared with the copper-mold-casting method. The corrosion resistance of this amorphous steel in sulfuric-acid solutions was determined by electrochemical measurements. The passive film formed on the surface of the alloy after immersion in the 0.5-mol/l H₂SO₄ solution for 1 week was analyzed by X-ray photoelectron spectroscopy (XPS). Electrochemical measurements show that the corrosion resistance of the amorphous steel in the 1 mol/l-H₂SO₄ solution is superior to a stainless steel (SUS 321), and is almost the same as Ti6Al4V, which shows that the amorphous steel has an excellent corrosion resistance in sulfuric-acid solutions. As the concentration of the sulfuric-acid solutions increases from 0.5 mol/l to 4 mol/l, the corrosion resistance of the amorphous steel decreases. The XPS result reveals that a bilayer structure of protective film formed on the surface of the amorphous steel in a H₂SO₄ solution. The compositions of the inner part of the film are MoO₂, Cr₂O₃, CoO, and FeO, and those of the outer film are MoO₃, Cr(OH)₃, Co(OH)₂, and Fe(OH)₃.     

Effect of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Concentration on Density and Structure of (CaO-SiO<Subscript>2</Subscript>)-xAl<Subscript>2</Subscript>O<Subscript>3</Subscript> Slag

The effect of Al₂O₃ concentration on the density and structure of CaO-SiO₂-Al₂O₃ slag was investigated at multiple Al₂O₃ mole percentages and at a fixed CaO/SiO₂ ratio of 1. The experiments were conducted in the temperature range of 2154 K to 2423 K (1881 °C to 2150 °C) using the aerodynamic levitation technique. In order to understand the relationship between density and structure, structural analysis of the silicate melts was carried out using Raman spectroscopy. The density of each slag sample investigated in this study decreased linearly with increasing temperature. When the Al₂O₃ content was less than 15 mole pct, density decreased with increasing Al₂O₃ content due to the coupling of Si (Al), whereas above 20 mole pct density of the slag increased due to the role of Al³⁺ ion as a network modifier.     

High-temperature deformation behavior of coarse- and fine-grained MoSi<Subscript>2</Subscript> with different silica contents

The elevated-temperature deformation behavior of polycrystalline molybdenum disilicide (MoSi₂), in the range of 1000 °C to 1350 °C at the strain rates of 10⁻³, 5×10⁻⁴, or 10⁻⁴ s⁻¹, has been studied. The yield strength, post-yield flow behavior comprising strain hardening and serrations, as well as some of the deformation microstructures of reaction-hot-pressed (RHP) MoSi₂ samples, processed by hot pressing an elemental Mo + Si powder mixture and having a grain size of 5 μm and oxygen content of 0.06 wt pct, have been compared with those of samples prepared by hot pressing of commercial-grade Starck MoSi₂ powder, with a grain size of 27 μm and oxygen content of 0.89 wt pct. While the fine-grained RHP MoSi₂ samples have shown higher yield strength at relatively lower temperatures and higher strain rates, the coarse-grained Starck MoSi₂ has a higher yield at decreasing strain rates and higher temperatures. The work-hardening or softening characteristics are dependent on grain size, temperature, and strain rate. Enhanced dislocation activity and dynamic recovery, accomplished by arrangement of dislocations in low-angle boundaries, characterize the deformation behavior of fine-grained RHP MoSi₂ at a temperature of 1200 °C and above and are responsible for increased uniform plastic strain with increasing temperature. The silica content appears to be less effective in degrading the high-temperature yield strength if the grain size is coarse, but leads to plastic-flow localization and strain softening in Starck MoSi₂. Serrated plastic flow has also been observed in a large number of samples, mostly when deformed at specific combinations of strain rates and temperatures.