Microstructure Evolution in Nano-reinforced Ferritic Steel Processed By Mechanical Alloying and Spark Plasma Sintering

Oxide-dispersion strengthened ferritic steel was produced by high-energy attrition, leading to a complex nanostructure with deformed ferritic grains. After mechanical alloying, the powder was then consolidated by spark plasma sintering (SPS) using various thermo-mechanical treatments. Hot isostatic pressing (HIP) was also performed on the same powder for comparison. Above 1123 K (850 °C), SPS consolidation-induced heterogeneous microstructure composed of ultra-fine-grained regions surrounded by larger grains. Spatial distribution of the stored energy was measured in the bimodal microstructure using the Kernel average misorientation. In contrary to large recrystallized grains, ultra-fine grains are still substructured with low-angle grain boundaries. The precipitation kinetics of the nano-oxides during consolidation was determined by small-angle neutron scattering. Precipitation mainly occurred during the heating stage, leading to a high density of nanoclusters that are of prime importance for the mechanical properties. Other coarser titanium-enriched oxides were also detected. The multiscale characterization allowed us to understand and model the evolution of the complex microstructure. An analytical evaluation of the contributing mechanisms explains the appearance of the complex grain structure and its thermal stability during further heat treatments. Inhomogeneous distribution of plastic deformation in the powder is the major cause of heterogeneous recrystallization and further grain growth during hot consolidation. Then, the thermal stability of coherent nano-oxides is responsible for effective grain boundary pinning in recovered regions where the driving pressure for recrystallization is lowered. This scenario is confirmed in both SPSed and HIPed materials.     

Mechanical Behavior of Al-SiC Nanocomposites Produced by Ball Milling and Spark Plasma Sintering

Al-SiC nanocomposites were prepared by high energy ball milling of mixtures of pure Al and 50-nm-diameter SiC nanoparticles, followed by spark plasma sintering. The final composites had grains of approximately 100 nm dimensions, with SiC particles located mostly at grain boundaries. The samples were tested in uniaxial compression by nano- and microindentation in order to establish the effect of the SiC volume fraction, stearic acid addition to the powder, and the milling time on the mechanical properties. The results are compared with those obtained for pure Al processed under similar conditions and for AA1050 aluminum. The yield stress of the nanocomposite with 1 vol pct SiC is more than ten times larger than that of AA1050. The largest increase is due to grain size reduction; nanocrystalline Al without SiC and processed by the same method has a yield stress seven times larger than AA1050. Adding 0.5 vol pct SiC increases the yield stress by an additional 47 pct, while the addition of 1 vol pct SiC leads to 50 pct increase relative to the nanocrystalline Al without SiC. Increasing the milling time and adding stearic acid to the powder during milling lead to relatively small increases of the flow stress. The hardness measured in nano- and microindentation experiments confirms these trends, although the numerical values of the gains are different. The stability of the microstructure was tested by annealing samples to 423 K and 523 K (150 °C and 250 °C) for 2 hours, in separate experiments. The heat treatment had no effect on the mechanical properties, except when treating the material with 1 vol pct SiC at 523 K (250 °C), which led to a reduction of the yield stress by 13 pct. The data suggest that the main strengthening mechanism is associated with grain size reduction, while the role of the SiC particles is mostly that of stabilizing the nanograins.     

化学浸润法氧化物弥散强化铁素体合金的静态再结晶

研究了用化学浸润法(CS)进行氧化物弥散强化(ODS)的铁素体合金形变后在退火过程中的组织变化.结果表明:合金的再结晶温度在750~780 ℃之间;形变量高的合金退火后能获得细小均匀的晶粒;弥散相能有效钉扎初次再结晶完成后晶粒尺寸在临界尺寸D_lim以下的晶界;弥散强化相Y₂Ti₂O₃在形变和退火过程中是稳定的.     

Characterization of Oxide Dispersed AlCoCrFe High Entropy Alloy Synthesized by Mechanical Alloying and Spark Plasma Sintering

The present study deals with phase evolution of oxide dispersed AlCoCrFe high entropy alloy during mechanical alloying and spark plasma sintering. Mechanical alloying of AlCoCrFe resulted in a single BCC phase. However, ordering of BCC phase with evolution of chromium carbide and sigma phase were observed after spark plasma sintering. High hardness of 1,050 ± 20 HV₁ and 1,070 ± 20 HV₁ was observed for AlCoCrFe high entropy alloy without and with oxide dispersion, respectively. Significant contribution from solid solution strengthening effect in high entropy alloys appears to have overwhelmed the effect of oxide dispersion on hardness.     

Enhanced Electrical and Mechanical Properties of Alumina-Based TiC Composites by Spark Plasma Sintering

Alumina composites incorporating with 0, 5, 10 15, 20, and 25 vol pct of TiC were consolidated by the spark plasma sintering at 1673 K (1400 °C). The effects of increasing TiC compositions on electrical and mechanical properties of the composites were investigated at room temperature. The dc electrical conductivity behavior demonstrates a transition from insulator to conductor around 12.5 vol pct of TiC in the framework of percolation theory. The conductivity attains a maximum value of ≈230 S/m at 25 vol pct of TiC sufficient to machine the composite by electro discharging machining. The Vickers hardness and fracture toughness of the composites increase with the addition of TiC vol pct, whereas elastic modulus decreases. The results indicate that crack deflection, crack bridging, and crack branching by the TiC particles are responsible for the significantly improved fracture toughness of the composites.     

Evaluation of Thermal and Mechanical Behavior of CuNiCoZnAl High-Entropy Alloy Fabricated Using Mechanical Alloying and Spark Plasma Sintering

Thermal behavior investigation of CuNiCoZnAl high-entropy alloy powder produced by mechanical alloying indicated that a FCC single-phase solid solution transformed into two new phases at 500 °C. Despite this phase transformation, no indication of intermetallic compounds or amorphous phases was detected. Heat treatment of the high-entropy alloy was then carried out for 2 hours, and the nanocrystalline structure of heat-treated milled powder was retained up to 1000 °C. Besides, grain growth of CuNiCoZnAl high-entropy alloy powder at high homologous temperatures (> 0.6 T_m) was studied, and sluggish grain growth of the powder was observed clearly. Consolidation of the alloy powder was performed by spark plasma sintering at 800 °C, and a sample with porosity of 6.87 pct and density of 7.32 g cm⁻³ was achieved. Elastic moduli, Vickers microhardness, and fracture toughness of the bulk sample were measured as 186 ± 17 GPa, 599 ± 31 HV, and 4.45 MPa m^0.5, respectively. The evaluation of wear behavior indicated that the dominant wear mechanism was adhesive wear. Moreover, tribochemical wear (oxidation) was found to be the minor wear mechanism. The present study revealed that CuNiCoZnAl high-entropy alloy has the potential to be used in many applications that high hardness and low elastic moduli are favorable.

     

Fabrication of Ni-Ti Alloy by Self-Propagating High-Temperature Synthesis and Spark Plasma Sintering Technique

This work is focused on the possibilities of preparing Ni-Ti46 wt pct alloy by powder metallurgy methods. The self-propagating high-temperature synthesis (SHS) and combination of SHS reaction, milling, and spark plasma sintering consolidation (SPS) are explored. The aim of this work is the development of preparation method with the lowest amount of undesirable phases (mainly Ti₂Ni phase). The SHS with high heating rate (approx. 200 and 300 K min^?1) was applied. Because the SHS product is very porous, it was milled in vibratory disk milling and consolidated by SPS technique at temperatures of 1173 K, 1273 K, and 1373 K (900 °C, 1000 °C, and 1100 °C). The microstructures of samples prepared by SHS reaction and combination of SHS reaction, milling, and SPS consolidation are compared. The changes in microstructure with increasing temperature of SPS consolidation are observed. Mechanical properties are tested by hardness measurement. The way to reduce the amount of Ti₂Ni phase in structure is leaching of powder in 35 pct hydrochloric acid before SPS consolidation.     

Evaluation of Microstructure and Mechanical Properties of Nano-Y2O3-Dispersed Ferritic Alloy Synthesized by Mechanical Alloying and Consolidated by High-Pressure Sintering

In this study, an attempt has been made to synthesize 1.0 wt pct nano-Y₂O₃-dispersed ferritic alloys with nominal compositions: 83.0 Fe-13.5 Cr-2.0 Al-0.5 Ti (alloy A), 79.0 Fe-17.5 Cr-2.0 Al-0.5 Ti (alloy B), 75.0 Fe-21.5 Cr-2.0 Al-0.5 Ti (alloy C), and 71.0 Fe-25.5 Cr-2.0 Al-0.5 Ti (alloy D) steels (all in wt pct) by solid-state mechanical alloying route and consolidation the milled powder by high-pressure sintering at 873 K, 1073 K, and 1273 K (600°C, 800°C, and 1000°C) using 8 GPa uniaxial pressure for 3 minutes. Subsequently, an extensive effort has been undertaken to characterize the microstructural and phase evolution by X-ray diffraction, scanning and transmission electron microscopy, and energy dispersive spectroscopy. Mechanical properties including hardness, compressive strength, Young’s modulus, and fracture toughness were determined using micro/nano-indentation unit and universal testing machine. The present ferritic alloys record extraordinary levels of compressive strength (from 1150 to 2550 MPa), Young’s modulus (from 200 to 240 GPa), indentation fracture toughness (from 3.6 to 15.4 MPa√m), and hardness (from13.5 to 18.5 GPa) and measure up to 1.5 through 2 times greater strength but with a lower density (~7.4 Mg/m³) than other oxide dispersion-strengthened ferritic steels (<1200 MPa) or tungsten-based alloys (<2200 MPa). Besides superior mechanical strength, the novelty of these alloys lies in the unique microstructure comprising uniform distribution of either nanometric (~10 nm) oxide (Y₂Ti₂O₇/Y₂TiO₅ or un-reacted Y₂O₃) or intermetallic (Fe₁₁TiY and Al_9.22Cr_2.78Y) particles' ferritic matrix useful for grain boundary pinning and creep resistance.     

Effect of Y2O3 on Spark Plasma Sintering Kinetics of Nanocrystalline 9Cr-1Mo Ferritic Oxide Dispersion-Strengthened Steels

Nanocrystalline mechanically alloyed powders of 9Cr-1Mo ferritic steels with and without yttria dispersoids were densified using spark plasma sintering (SPS) to near-theoretical density at a temperature of 1073 K (800 °C). Studies on densification behaviour revealed that steels with dispersoids densified faster when compared to Fe-9Cr-1Mo steel. The evaluation of densification mechanisms during SPS reveals that grain boundary and lattice diffusion to be predominant at relative densities ranging from >0.7 to 0.9 in both the alloys.     

Effects of Annealing Temperature on Microstructure and Tensile Properties in Ferritic Lightweight Steels

An investigation was conducted into the effects of annealing temperature on microstructure and tensile properties of ferritic lightweight steels. Two steels were fabricated by varying the C content, and were annealed at 573 K to 1173 K (300 °C to 900 °C) for 1 hour. According to the microstructural analysis results, κ-carbides were formed at about 973 K (700 °C), which was confirmed by equilibrium phase diagrams calculated from a THERMO-CALC program. In the steel containing low carbon content, needle-shaped κ-carbides were homogeneously dispersed in the ferrite matrix, whereas bulky band-shaped martensites were distributed in the steel containing high carbon content. In the 973 K (700 °C)-annealed specimen of the steel containing high carbon content, deformation bands were formed throughout the specimen, while fine carbides were sufficiently deformed inside the deformation bands, thereby resulting in the greatest level of strength and ductility. These results indicated that the appropriate annealing treatment of steel containing high carbon content was useful for the improvement of both strength and ductility over steel containing low carbon content.     

Microstructure,Mechanical Properties,and Sliding Wear Behavior of Oxide-Dispersion-Strengthened FeMnNi Alloy Fabricated by Spark Plasma Sintering

Metallurgical and Materials Transactions A - The face-centered-cubic (fcc) CoCrFeMnNi high-entropy alloy suffers from low strength and wear resistance at ambient temperature. Herein, we developed a...     

用于超临界水堆燃料包壳的ODS铁素体钢的研究进展

 超临界水堆具有热效率高、系统简化、成本低等优点,成为第四代核反应堆中优先发展的堆型。ODS铁素体钢由于其优异的高温力学性能和良好的抗辐照能力成为超临界水堆包壳最有希望的候选材料。本文旨在回顾ODS铁素体钢制造工艺,包括机械合金化参数的优化,热处理工艺的选择以消除力学性能上的各向异性。根据超临界水堆包壳的服役条件,结合最新的实验数据,对ODS铁素体钢的高温力学性能、在超临界水中的耐腐蚀性以及中子辐照稳定性进行了总结和展望。     

放电等离子烧结的超细纯碳化钨的组织与性能

利用放电等离子烧结技术得到了近全致密的无粘结相超细纯碳化钨材料。烧结前后平均粒径达200nm的超细组织基本维持不变。该材料的硬度明显超过了常规的碳化钨基硬质合金，可以用作优异的硬质材料。     

Role of Microstructure and Temperature on the Tensile Fracture Behavior of Oxide Dispersion Strengthened 18Cr Ferritic Steel

The tensile fracture behavior of oxide dispersion strengthened 18Cr (ODS-18Cr) ferritic steels milled for varying times was studied along with the oxide-free 18Cr steel (NODS) at 25, 200, 400, 600, and 800 °C. At all the test temperatures, the strengths of ODS–18Cr steels increased and total elongation decreased with the duration of milling time. Oxide dispersed 18Cr steel with optimum milling exhibited enhanced yield strength of 156 pct at room temperature and 300 pct at 800 °C when compared to oxide-free 18Cr steel. The ductility values of ODS-18Cr steels are in the range 20 to 35 pct for a temperature range 25 to 800 °C, whereas NODS alloy exhibited higher ductility of 37 to 82 pct. The enhanced strength of ODS steels when compared to oxide-free steel is due to the development of ultrafine grained structure along with nanosized dispersion of complex oxide particles. While the pre-necking elongation decreased with increasing temperature and milling time, post-necking elongation showed no change with the test temperature. Fractographic examination of both ODS and NODS 18Cr steel fractured tensile samples, revealed that the failure was in ductile fracture mode with distinct neck and shear lip formation for all milling times and at all test temperatures. The fracture mechanism is in general followed the sequence; microvoid nucleation at second phase particles, void growth and coalescence. The quantified dimple sizes and numbers per unit area were found to be in linear relation with the size and number density of dispersoids. It is clearly evident that even nanosized dispersoids acted as sites for microvoid nucleation at larger strains and assisted in dimple rupture.

     

Study of TRIP-Aided Bainitic Ferritic Steels Produced by Hot Press Forming

A study is reported to produce high strength ductile steels by controlled cooling following hot press forming, instead of quenching, as is practiced in the traditional press hardened steels. Heat treatments of several specially designed low carbon steels were carried out by interrupting the fast cooling from the austenization temperature at temperatures between T ₀ and Ms and then cooling in controlled rates to room temperature. The effect of the interrupt temperature and the cooling rate afterward on the microstructures and tensile properties was studied. The microstructures were characterized using dilatometry, optical microscopy, X-ray diffraction, and TEM. A multi-phase microstructure including bainite, martensite, and retained austenite was obtained in the simulated hot press forming process. Volume fraction bainite was found to increase with an increase in interrupt temperature and a decrease in cooling rate. Structure–property correlations of the studied steels heat treated at different conditions were developed. Improved tensile properties were obtained by controlling the interrupt temperature and cooling rate which produced an optimum bainite content of 60 to 75 pct and retained austenite. Unfortunately, the bainite in the simulated samples was not completely carbide free even though the steels contained about 1.6 wt pct of Si.     

Structure and Magnetic Properties of Sm2Fe17Nx Sintering Magnets Prepared by Spark Plasma Sintering

Bulk Sm2Fe17Nx sintering magnet was fabricated by spark plasma sintering(SPS) technique. The effects of sintering pressure and sintering temperature on the magnetic properties of the Sm2Fe17Nx magnet were investigated. As a result, the density of the magnet is obviously improved with the increase of sintering pressure, but the coercivity drops since Sm2Fe17Nx has decomposed into SmN, α-Fe and N2. When sintering temperature was only above 200 ℃ under 1 GPa sintering pressure, the coercivity even begins to decrease, which indicates that high pressure promotes the decomposition of the Sm2Fe17Nx at lower temperature. The decomposition is also proved by the decrease of nitrogen and increase of α-Fe in the magnets.