Microstructural changes upon annealing in ODS-strengthened ultrafine grained ferritic steel

In this study, the stability of grain size and oxide nanoparticles in the ODS steel upon annealing at high temperature (650–1350 °C) has been evaluated. The ODS Fe–Cr–W–Ti–Y₂O₃ steel has been manufactured by powder metallurgy, consolidated by hot isostatic pressing and processed by hydrostatic extrusion. Such a processing brings about ultrafine grain structure reinforced with oxide nanoparticles (few nm in diameter) and results in superior mechanical properties. The stability of nano-oxides has been analyzed by small angle X-ray scattering together with transmission electron microscopy. The results obtained revealed excellent thermal stability of ultrafine grained ODS ferritic steel, which was attributed to the resistance of oxides against coarsening.     

Relation between microstructure and Charpy impact properties of an elemental and pre-alloyed 14Cr ODS ferritic steel powder after hot isostatic pressing

This article describes the microstructure and Charpy impact properties of an Fe–14Cr–2W–0.3Ti–0.3Y₂O₃ oxide dispersion strengthened (ODS)-reduced activation ferritic (RAF) steel, manufactured either from elemental powders or from an Fe–14Cr–2W–0.3Ti pre-alloyed powder. ODS RAF steels have been produced by mechanical alloying of powders with 0.3 wt% Y₂O₃ nanoparticles in either a planetary ball mill or an attritor ball mill, for 45 and 20 h, respectively, followed by hot isostatic pressing (HIPping) at 1,150 °C under a pressure of 200 MPa for 4 h and heat treatment at 850 °C for 1 h. It was found that the elemental ODS steel powder contains smaller particles with a higher specific surface area and a two times higher oxygen amount than the pre-alloyed ODS steel powder. After HIPping both materials exhibit a density higher than 99%. However, the pre-alloyed ODS steel exhibits a slightly better density than the elemental ODS steel, due to the reduced oxygen content in the former material. Charpy impact experiment revealed that the pre-alloyed ODS steel has a much larger ductile-to-brittle transition temperature (DBTT) (about 140 °C) than the elemental ODS steel (about 25 °C). However, no significant difference in the upper shelf energy (about 3.0 J) was measured. TEM and SEM–EBSD analyses revealed that the microstructure of the elemental ODS steel is composed of smaller grains with a larger fraction of high-angle grains (>15°) and a lower dislocation density than the pre-alloyed ODS steel, which explains the lower DBTT value obtained for the elemental ODS steel.     

Microstructure characterisation and tensile properties of 18Cr-4.5Al-0.3Zr- oxide dispersion strengthened steel

The 18Cr–4.5Al–0.3Zr–oxide dispersion strengthened (ODS) steel was fabricated by mechanical alloying (MA) and spark plasma sintering (SPS) technique. A microstructural characterisation was performed on an 18Cr–4.5Al–0.3Zr–ODS steel using high angle annual dark field (HAADF) and synchrotron small angle X-ray scattering (SAXS). HAADF and SAXS results showed that high-density nanoscale oxides are formed in 18Cr–4.5Al–0.3Zr–ODS steel. The oxides in the specimen can be roughly divided into two categories according to their compositions: (1) core/shell structure oxides with Al–O oxide cores and Y shells; (2) nm-scale trigonal-phase Y₄Zr₃O₁₂ oxides. In addition, tensile testing results revealed that the specimen exhibited better tensile strength and ductility as compared with another commercial ODS steels with similar composition.     

Feasibility of using Y2Ti2O7 nanoparticles to fabricate high strength oxide dispersion strengthened Fe–Cr–Al steels

Addition of Al can improve the corrosion resistance of oxide dispersion strengthened (ODS) steels. However, Al reacts with Y₂O₃ to form large Y–Al–O particles in the steels and deteriorates their mechanical properties. Herein, we successfully prepared Y₂Ti₂O₇ nanoparticles (NPs) by the combination of hydrogen plasma-metal reaction (HPMR) and annealing. Y₂Ti₂O₇ NPs with contents of 0.2 or 0.6 wt.% were then added into the Fe–14Cr–3Al–2W–0.35Ti (wt.%) steel to substitute the conventional Y₂O₃ NPs by mechanical alloying (MA). The Y₂Ti₂O₇ NPs transformed into amorphous-like structure after 96 h MA. They crystallized with a fine size of 7.4 ± 3.7 nm and shared a semi-coherent interface with the matrix after hot isostatic pressing (HIP) of the ODS steel with 0.6 wt.% Y₂Ti₂O₇. With the increasing Y₂Ti₂O₇ content from 0.2 to 0.6 wt.%, the tensile strength of the ODS steel increased from 1238 to 1296 MPa, which was much higher than that (949 MPa) of the ODS steel added with Y₂O₃. The remarkably improved mechanical properties of the Al-containing ODS steels were attributed to the increasing number density of Y₂Ti₂O₇ nanoprecipitates. Our work demonstrates a novel route to fabricate high performance ODS steels with both high mechanical strength and good corrosion resistance.     

Microstructure and mechanical properties of spark plasma sintered austenitic ODS steel

In this work, austenitic oxide dispersion strengthened (AODS) steel of composition Fe–16Cr–16Ni–1.5 W–0.21Ti–0.3Y₂O₃ (wt. %) was fabricated using two–stage ball milling followed by consolidation through spark plasma sintering (SPS). In the first–stage, mechanical alloying (MA) of ferritic powder and nano sized Y₂O₃ was carried out. This was followed by the addition of Ni in second–stage milling. SPS of the milled powder was carried out at 900, 950, 1000 and 1050 °C to explore the role of SPS temperature on density, microstructure as well as mechanical properties of the consolidated samples. A relative density of ～ 99% was obtained for samples sintered at 950 and 1000 °C. The as–sintered samples were subsequently solution annealed at 1075 °C for 2 h and water quenched. X–ray diffraction studies confirmed the presence of austenite in the consolidated and solution annealed samples. Electron back scatter diffraction analysis of solution annealed samples sintered at all the temperatures revealed a bimodal microstructure. The average grain size of 1.07 ± 0.72 µm was obtained for solution annealed samples sintered at 1000 °C. Yield strength and elongation of the same was measured as 851 MPa and 18%, respectively at room temperature. These values are the best combination of strength to elongation achieved on AODS alloys processed using MA and SPS, which makes this AODS steel much promising for high temperature applications.     

Effect of Zr on microstructure and mechanical properties of the Al–Cu–Er alloy

ABSTRACT

The microstructure and mechanical properties of the Al–4Cu–2.7Er–0.3Zr alloy were investigated. The precipitates of the L1₂ structured phase with sizes 37?±?12?nm were formed in lines and homogenously distributed inside the aluminium matrix after annealing at 605°C for 1?h. The as-rolled Al–4Cu–2.7Er–0.3Zr alloy developed an increased hardness after 1?h annealing at 100–550°C and 0.5–6?h annealing at 150–250°C due to precipitation of the Al₃(Er,Zr) phase. Addition of Zirconium improved the tensile properties relative to those of the Zr-free alloy by approximately 20?MPa: yield strength?=?273–296?MPa and ultimate tensile strength?=?296–328?MPa in the alloys annealed at 100–150°C.     

Interactions between Y2O3–Al mixture studied by solid-state reaction method

Interactions between Y₂O₃–Al mixture studied by solid-state reaction method were investigated in present paper. Interactions between Y₂O₃–Al mixture was characterized by differential thermal and thermogravimetric analyses and X-ray diffraction, Y₂O₃–Al mixture and yttrium aluminum garnet (YAG) powder as final reaction product were characterized by scanning electron microscopy. The results show Al is isolated with Y₂O₃ by aluminum oxide layer in air, and no opportunity of directional reaction between Y₂O₃–Al systems. With temperature increasing to ∼569 °C, aluminum partly turned into transitional aluminas, Y₂O₃ reacts with transitional aluminas instead of aluminum to form yttrium aluminum monoclinic (YAM) and yttrium aluminum perovkite (YAP) phases after calcination at 600 °C, 800 °C separately, and pure YAG powder is obtained after calcination at 1200 °C. From the point of view of reaction temperature, the reaction between Y₂O₃ and transitional aluminas is easier than that of Y₂O₃ and Al or α-Al₂O₃.     

Microstructural evolution of oxide-dispersion-strengthened Fe–Cr model steels during mechanical milling and subsequent hot pressing

Oxide-dispersion-strengthened (ODS) ferritic steels of Fe–9Cr–0.3Y₂O₃ and Fe–9Cr–0.2Ti–0.3Y₂O₃ (in mass) incorporating nanoscale oxide particles, were produced by mechanical milling (MM) followed by hot pressing (HP). Microstructural evolution of these two types of ODS steels were structurally characterized at each step of the elaboration processes by means of scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), and optical microscope. The observations of structure of the mixed powders and the nanoscale oxide particles in both ODS steels after MM indicate that the initial powders, coupled with the original yttria powders, get fractured by severe plastic deformation and ultrafine bcc grains (~20 nm) of the matrix and Y₂O₃ nanocrystals with irregular edges are formed during MM. The addition of titanium (Ti) promotes the refinement of bcc grains, Y₂O₃ nanocrystals and the formation of amorphous phase of Y₂O₃ during MM. TEM observations of these two Oxide-dispersion-strengthened (ODS) steels exhibit a very fine structure of micrometer-scale grains in which large number of nanoscale oxide particles are distributed after HP process. The observation of some unreinforced domains without the nanoscale oxide particles indicates that there still exist inhomogeneous areas, although the size of those oxide particles reaches nanoscale. Threshold stress of the HPped Fe–9Cr–0.2Ti–0.3Y₂O₃ steel with the relatively homogeneous dispersion was carefully evaluated on the basis of higher magnified images of the nanoscale oxide particles. Different values of threshold stress were obtained due to the various dispersions of the nanoscale oxide particles within different areas. That may be the reason why the threshold stress cannot be clearly obtained by the results of creep tests.     

Effects of post-annealing on the microstructure and mechanical properties of friction stir processed Al–Mg–TiO2 nanocomposites

Aluminum matrix nanocomposites were fabricated via friction stir processing of an Al–Mg alloy with pre-inserted TiO₂ nanoparticles at different volume fractions of 3%, 5% and 6%. The nanocomposites were annealed at 300–500 °C for 1–5 h in air to study the effect of annealing on the microstructural changes and mechanical properties. Microstructural studies by scanning and transmission electron microscopy showed that new phases were formed during friction stir processing due to chemical reactions at the interface of TiO₂ with the aluminum matrix alloy. Reactive annealing completed the solid-state reactions, which led to a significant improvement in the ductility of the nanocomposites (more than three times) without deteriorating their tensile strength and hardness. Evaluation of the grain structure revealed that the presence of TiO₂ nanoparticles refined the grains during friction stir processing while the in situ formed nanoparticles hindered the grain growth upon the post-annealing treatment. Abnormal grain growth was observed after a prolonged annealing at 500 °C. The highest strength and ductility were obtained for the nanocomposites annealed at 400 °C for 3 h.     

Influence of heat treatment on microstructure and adhesion of Al2O3 fiber-reinforced electroless Ni–P coating on Al–Si casting alloy

Influence of heat treatment regime on microstructure, phase composition and adhesion of Al₂O₃ fiber-reinforced Ni–P electroless coating on an Al–10Si–0.3 Mg casting alloy is investigated in this work. The pre-treated substrate was plated using a bath containing nickel hypophosphite, nickel lactate and lactic acid. Al₂O₃ fibers pretreated with demineralised water were placed into the plating bath. Resulting Ni–P–Al₂O₃ coating thickness was about 12 μm. The coated samples were heat treated at 400–550 °C/1–8 h. LM, SEM, EDS and XRD were used to investigate phase transformations. Adhesion of coating was estimated using scratch test with an initial load of 8.80 N. It is found that annealing at high temperatures (450 °C and above) leads to the formation of hard intermetallic products (namely Al₃Ni and Al₃Ni₂ phases) at the substrate–coating interface. However, as determined by the light microscopy and by the scratch test, these phases reduce the coating adhesion (compared to coatings treated by the optimal annealing regime 400 °C/1 h). The analysis of scratch tracks proves that fiber reinforcement significantly reduces the coating scaling. However, due to the formed intermetallic sub-layers, partial coating delamination may occur on the samples annealed at 450 °C and above.     

Al–Cu–Fe coatings manufactured by the flame spraying process

Two-hour milled (activated) Al–20Cu–15Fe (at%) powders were subjected to annealing at 600°C for 1?h. The phase and microstructural evolutions were characterized by X-ray diffractometry and scanning electron microscopy. Al₇Cu₂Fe and Al₆₀Cu₃₀Fe₁₀ phases were formed after annealing. Both annealed and milled powders were consolidated using the flame spraying process. In both cases, FeAl(Cu) was the major phase while some oxides and α-Fe(Al,Cu) were also found. The coating produced from the milled powder was severely cracked and showed higher oxide content. The coating prepared from the annealed powder showed better quality. It was annealed at 600°C for 1?h to investigate the thermal stability of the various phases. All phases persevered after annealing while the Fe₂Al₅ phase was formed as a new phase.     

Effect of post deposition reduction treatment of YIG thin films on stabilizing cubic garnet phase

Yttrium iron garnet thin films have been prepared by low pressure metallo-organic chemical vapour deposition method (MOCVD). Dipivaloyl methanates of yttrium and iron have been used as the precursors in the MOCVD growth of the garnet films. Post deposition O₂ annealing at 900°C is required to form a garnet phase which also shows orthoferrite and component Y₂O₃ and α-Fe₂O₃ phases. We show that a partial H₂ reduction treatment minimizes secondary phases and stabilizes the garnet phase. These treatments also enhance the magnetic properties considerably. Paper presented at the poster session of MRSI AGM VI, Kharagpur, 1995     

Effect of Zr on microstructure and mechanical property of dispersion-strengthened Pt-20Rh

Dispersion-strengthened Pt-20Rh was designed and prepared by powder metallurgy-internal oxidation-sintering. After rolling and annealing, the microstructures, mechanical properties at room temperature and 1000?°C were tested and analysed. Results indicate that the dispersion-strengthened Pt-20Rh alloy consists of Pt and Rh solid solution, Y₂O₃ and ZrO₂. It has a stabilised grain structure at 1000?°C. As the Zr content increases, the strengths at room temperature and high temperature are greatly improved. ZrO₂ particles can pin up and block the movement of dislocations, making it possible to enhance the strength. When Zr content is 0.3?wt-%, the room temperature and 1000?°C tensile strengths are up to their maximum, i.e. 555 and 149?MPa, respectively.     

Luminescence and crystallinity of flame-made Y2O3:Eu3+ nanoparticles

Cubic and/or monoclinic Y₂O₃:Eu³⁺ nanoparticles (10–50 nm) were made continuously without post-processing by single-step, flame spray pyrolysis (FSP). These particles were characterized by X-ray diffraction, nitrogen adsorption and transmission electron microscopy. Photoluminescence (PL) emission and time-resolved PL intensity decay were measured from these powders. The influence of particle size on PL was examined by annealing (at 700–1300°C for 10 h) as-prepared, initially monoclinic Y₂O₃:Eu³⁺ nanoparticles resulting in larger 0.025–1 μm, cubic Y₂O₃:Eu³⁺. The influence of europium (Eu³⁺) content (1–10 wt%) on sintering dynamics as well as optical properties of the resulting powders was investigated. Longer high-temperature particle residence time during FSP resulted in cubic nanoparticles with lower maximum PL intensity than measured by commercial micron-sized bulk Y₂O₃:Eu³⁺ phosphor powder. After annealing as-prepared 5 wt% Eu-doped Y₂O₃ particles at 900, 1100 and 1300°C for 10 h, the PL intensity increased as particle size increased and finally (at 1300°C) showed similar PL intensity as that of commercially available, bulk Y₂O₃:Eu³⁺ (5 μm particle size). Eu doping stabilized the monoclinic Y₂O₃ and shifted the monoclinic to cubic transition towards higher temperatures.     

Effect of annealing on microstructural and optoelectronic properties of nanocrystalline TiO2 thin films

In this study, semi-transparent nanostructured titanium oxide (TiO₂) thin films have been prepared by sol–gel technique. The titanium isopropoxide was used as a source of TiO₂ and methanol as a solvent and heat treated at 60°C. The as prepared powder was sintered at various temperatures in the range of 400–700°C and has been deposited onto a glass substrate using spin coating technique. The effect of annealing temperature on structural, morphological, electrical and optical properties was studied by using X-ray diffraction (XRD), high resolution transmittance electron microscopy (HRTEM), atomic force microscopy (AFM), scanning electron microscopy (SEM), dc resistivity measurement and optical absorption studies. The XRD measurements confirmed that the films grown by this technique have good crystalline nature with tetragonal-mixed anatase and rutile phases and a homogeneous surface. The HRTEM image of TiO₂ thin film (annealed at 700°C) showed grains of about 50–60?nm in size with aggregation of 10–15?nm crystallites. Electron diffraction pattern shows that the TiO₂ films exhibited a tetragonal structure. SEM images showed that the nanoparticles are fine and varies with annealing temperature. The optical band gap energy decreases with increasing annealing temperature. This means that the optical quality of TiO₂ films is improved by annealing. The dc electrical conductivity lies in the range of 10^?6 to 10^?5?Ω?cm^?1 and it decreases by the order of 10 with increase in annealing temperature from 400°C to 700°C. It is observed that the sample Ti700°C has a smooth and flat texture suitable for different optoelectronic applications.     

Ferromagnetism and Morphology of Annealed Fe2O3/CoXOY/ZnO Thin Films

We have studied thermal solid‐state reactions in the Fe₂O₃/Co_XO_Y/ZnO thin film systems grown using the atomic layer deposition technique. The compound produced after annealing at 700 °C is found to be a complex mixture of three different spinel phases: ZnCo₂O₄, CoFe₂O₄, and ZnFe₂O₄. The magnetic properties of the compound strongly depend on the atomic ratio of Fe³⁺ and Co²⁺ atoms, which can be set by choosing the corresponding thicknesses of the Fe₂O₃ and Co_XO_Y films. In addition, we also find a formation of 100 nm voids at the interface between Fe–Co–Zn–O compound and remaining ZnO film after 1h annealing at 700 °C in argon atmosphere. The formation of these voids shows indirectly the preferential outward diffusion of Zn²⁺ ions from ZnO into the Fe₂CoO₄ phase layer what we prove via our magnetic measurements.     

Study of the Crystal Structures of New Buffer Materials Bi1?xYxO1.5

Bismuth based oxides, formed by bismuth oxide doped with the yttrium or lanthanum element, have been widely studied for their high ionic conductivities and other applicable properties. Recently, they were used as buffer layers for film superconductors and have shown a promising future. But the detailed information of their structures and properties has not been fully understood. In this work, the series samples of Bi_1−x Y _x O_1.5 (x=0.2, 0.3, 0.4, and 0.5, respectively) were prepared. The crystalline structures of them were determined by X-ray powder diffraction and the data were analyzed by Rietveld refinement method. Two phases, face centered cubic (FCC) and rhombohedral structures, were observed. When annealed at 1,000 °C, the samples are FCC structure. But for Bi_0.8Y_0.2O_1.5, annealed at 650 °C, the sample shows a rhombohedral structure. The change of the structures of the samples were studied and discussed.     

Effect of Y<Subscript>2</Subscript>O<Subscript>3</Subscript> stabilizer content and annealing on the structural transformations of ZrO<Subscript>2</Subscript>

The structure of partially stabilized zirconia crystals has been studied by transmission electron microscopy before and after annealing. Structural characterization of Y₂O₃-doped (2.8 to 4 mol %) zirconia before annealing showed that all of the samples consisted of twin domains whose size was dependent on the stabilizer content. Annealing at 2100°C increased the domain size in the composition range 2.8–3.7 mol % Y₂O₃ and reduced it at 4 mol % Y₂O₃. These structural changes allowed us to determine the position of the representative point relative to the phase boundary in the equilibrium phase diagram of the system.     

Vibrational spectroscopic studies on crystallisation of sol–gel derived thin films of calcia–alumina binary compound

An optimized sol–gel process has been developed to produce homogeneous thin films of calcium aluminate binary (12CaO·7Al₂O₃) compound, on magnesium oxide substrates via spin coating. Fourier transform infrared and Raman spectroscopies have been employed to investigate the effect of annealing temperature and duration on the phase transformations in the films. Heat treatment at 1,300 °C under air atmosphere for 2 h produced single-phase 12CaO·7Al₂O₃ films. However, annealing at a lower temperature of 1,100 °C in air for a period of 4 h in total resulted in the crystallization of 5CaO·3Al₂O₃ rather than 12CaO·7Al₂O₃. The X-ray photoelectron spectrum of the thin film annealed at 1,300 °C corresponds to the binding energies of C12A7 compound. The annealing temperature of 1,300 °C for 2 h is found to be sufficient for formulating single phase calcia–alumina binary films in correct stoichiometric ratio of 12:7.     

Alloying behavior of gold,Au-Ge and Au-Ge-Ni on GaAs

The alloying behavior of gold, Au-Ge and Au-Ge-Ni films on GaAs has been studied after furnace annealing at 350 °C, 425 °C and 450 °C for 15 min, 0.5 min and 15 min respectively. Rutherford backscattering reveals that gold from Au-Ge films diffuses into the GaAs at a much lower temperature than that from gold and Au-Ge-Ni films. Transmission electron microscopy analysis reveals the presence of β-Ga₂O₃ in the 450 °C annealed specimens. In addition to this, the presence of Au₇Ga₂ and metastable γ-(Au-Ge) phases was identified in annealed Au-Ge films. Scanning electron micrographs of annealed samples show black patches which were found to be gold deficient compared with the light-gray areas. The surface morphology of Au-Ge-Ni films after alloying is more uniform than that of Au-Ge films.