Effect of second phase particles on grain refinement during equal-channel angular pressing of an Al-Mg-Mn alloy

The process of grain refinement under severe plastic deformation was examined in an Al-5.4% Mg-0.5% Mn-0.1% Zr alloy, which was subjected to equal-channel angular pressing (ECAP) in the strain interval from 1 to 12 at a temperature of ∼300 °C. It was shown that the size and distribution of the second phase particles precipitated under homogenization annealing strongly affect grain refinement. Extensive grain refinement under ECAP was provided by a dispersion of Al₆Mn particles with an average size of ∼25 nm that precipitated during the homogenization annealing at an intermediate temperature. The fully recrystallized structure with an average crystallite size of ∼0.55 μm evolves through continuous dynamic recrystallization. In contrast, homogenization annealing at a high temperature leads to the formation of coarse Al₆Mn particles with a plate-like shape. Under further ECAP, the formation of coarse recrystallized grains takes place in this material due to the discontinuous growth of recrystallized grains during the inter-pass annealing between the ECAP passes. The role of second phases in grain refinement is discussed in terms of pinning and driving forces for recrystallization.     

Nanocrystalline FeAl intermetallic produced by mechanical alloying followed by hot-pressing consolidation

In the present study mechanical alloying followed by hot-pressing consolidation has been used to obtain bulk nanocrystalline FeAl intermetallic compound. Nanocrystalline powder of Fe(Al) solid solution was the product of ball milling. This powder was sintered at 1000 °C for 180 s under a pressure of 7.7 GPa. Structural investigations of the consolidated material revealed that ordering of the Fe(Al) and its transformation into FeAl intermetallic occur during sintering and that the mean crystallite size of FeAl is 23 nm. The microhardness of the produced material is 1235 HV0.2, its density is 99.8% of theoretical value and its open porosity is 0%. The results obtained show that the quality of compaction with preserving nanometric grain size of the FeAl intermetallic is satisfactory and its microhardness is relatively high.     

Structure, mechanical properties and oxidation behaviour of arc-evaporated NbAlN hard coatings

Nb_1 − xAl_xN hard coatings were synthesised by cathodic arc-evaporation in order to study the influence of the Al concentration on crystal structure, mechanical properties and oxidation resistance. Structural investigations by X-ray diffraction revealed a transition from the face-centered cubic structure of δ-NbN to the wurtzite structure of AlN at x = 0.45… 0.56 depending on the deposition parameters. The maximum values of the mechanical properties like hardness and residual stress obtained by nanoindentation and biaxial stress temperature measurements, respectively, were found for the coatings with cubic structure and generally decrease with increasing Al content. On the other hand, higher Al concentrations are beneficial in terms of oxidation resistance as shown by annealing experiments in ambient air. The onset temperature for oxidation rises from 600 to 700 °C for Nb_0.73Al_0.27N to above 800 °C for Nb_0.29Al_0.71N regardless of changes in the crystal structure.     

Preliminary investigations on the Mg–Al–Zn/Al laminated composite fabricated by equal channel angular extrusion

In order to utilize the advantage of low density and overcome the disadvantages of poor corrosion resistance and low strength, the laminated composites of Mg alloys fabricated by different methods have attracted extensively attentions. In this paper, the equal channel angular extrusion (ECAE), which has been widely used to fabricate ultrafine grain bulk materials, was introduced to fabricate the Mg–3Al–1Zn/Al (AZ31/Al) laminated composites at different temperatures. After fabrication and annealing treatment at different temperatures, the microstructural evolution and phase constitution near the joining interface of AZ31/Al composites were evaluated using optical and scanning electron microscope as well as X-ray diffraction (XRD). The results indicated that the higher annealing temperature promoted the formations of thicker bonding layers and more reaction phases near the joining interface, which mainly included Mg₂Al₃ and Mg₁₇Al₁₂ phases. The AZ31/Al laminated composite fabricated at 300 °C revealed thicker diffusion layer than that fabricated at 200 °C after anneal under the same condition, and the appropriate technological parameters of fabricating AZ31/Al laminated composites were also discussed.     

The effect of Cu and Zn on the phase stability of L12 Al3Hf intermetallic compound synthesized by mechanical alloying

Elemental powders of Al and Hf were mechanically alloyed to produce L1₂ Al₃Hf powder with a nanocrystalline structure. The effect of the addition of ternary elements on the mechanical alloying behavior and the thermal stability of L1₂ phase was investigated. The start and finish temperatures of the phase transformation from L1₂ to D0₂₃ varied as a function of time and temperature in binary and ternary alloys. L1₂ Al₃Hf alloy was readily prepared by mechanical alloying for 6 h. It is thought that the homogeneous distribution of Al and Hf and following formation of the L1₂ phase are related with the attainment of the ultra-fine grain size of the powder. However, L1₂ phase was formed in the (Al+12.5 at.% M)₃Hf (M=Cu, Zn) alloys after 10 hours milling. The delayed formation of L1₂ phase in the ternary alloys was related to the retardation of the microstructural evolution or grain size refinement. The start temperature of the L1₂ to D0₂₃ phase transformation in the binary Al₃Hf alloy was only about 650 K, but it was increased to about 970 and 1170 K with the addition of 10 at.% Cu and 12.5 at.% Zn, respectively. Their grain size was less than 20 nm after 20 min heat treatment at each temperature. The start temperature of the phase transformation was not significantly affected by annealing time but the finish temperature of the transformation was decreased significantly with increasing annealing time. It is worth noting that the results in this study will be presented as useful data for the various consolidation processes of L1₂ nanocrystalline Al₃Hf powder.     

Structural and mechanical properties of Fe–Al compounds: An atomistic study by EAM simulation

The structural properties, formation enthalpies, and mechanical properties of Fe–Al compounds (FeAl, Fe₂Al, Fe₃Al, FeAl₂, FeAl₃ and Fe₂Al₅) are studied by using embedded-atom method (EAM) which is acquired by Mobius lattice inversion. The potential is transferrable and therefore does well for studying different Fe–Al compounds. The calculated lattice parameters and cohesive energies of Fe–Al compounds agree with the experimental and some EAM results. According to elastic constants restrictions, all the six Fe–Al compounds are mechanically stable. The calculated bulk moduli of the compounds increase with the increasing Fe concentration. Furthermore, results showed that FeAl, Fe₃Al, FeAl₃, FeAl₂, Fe₂Al₅ have lower ratios of shear modulus to bulk modulus and Fe₂Al has higher ratio.     

Features of intermetallic compounds in aluminized steels formed using aluminum foil

Foil aluminizing of steel, wherein Al diffuses to the base steel material by diffusion treatment after hot pressing of the aluminum foil at a lower temperature than the melting point, was performed in this study. Alloy layers formed by diffusion at temperatures ranging from 700 to 1000 °C were investigated, and their features were compared with those of hot-dip aluminized steel. In hot-dip aluminizing, an intermediate Fe₂Al₅ layer was formed between the aluminum layer and the base steel during aluminum coating before the diffusion treatment. In contrast, the coating layer of the foil-aluminized steel specimen after diffusion bonding of the aluminum foil consisted only of the Al layer. An Fe₂Al₅ layer, an FeAl layer and an Al diffused layer were formed in both the aluminized specimens subsequent to the diffusion treatment. The numbers of voids formed in the Fe₂Al₅ layer and at the FeAl/Al diffused layer interface of the foil-aluminized specimens are smaller than those for hot-dip aluminizing. Moreover, the FeAl and Al diffused layers are formed with a greater thickness in the foil-aluminized steel under identical diffusion conditions. The Al concentration in hot-dip aluminized steel decreased in stages from the surface to the base steel, whereas, in the foil-aluminized steel, it decreased gradually. The Fe₂Al₅/base steel interface in the foil-aluminized steel was thus indistinct, and cross-sectional hardness also decreased gradually.     

Producing nanocrystalline bulk Mg-3Al-Zn alloy by powder metallurgy assisted hydriding-dehydriding

Nanocrystalline bulk Mg-3Al-Zn alloy with an average grain size of 48 nm has been prepared by powder metallurgy assisted hydriding-dehydriding. Evolutions of nanograined structure powders and bulk alloy have been investigated by TEM, SEM and XRD, respectively. The results showed that by milling in hydrogen for 60 h, as-hydriding powder possessed an average grain size of 5.9 nm. After a subsequent process of desorption-recombination treatment (at 350 °C) and consolidation process (extruded at 200 °C) resulted in bulk samples with an average crystallite size of 48 nm and MgH₂ was fully turned into Mg. The consolidated samples of 60 h milled powder had a final density of 1.77663 ± 0.006 g/cm³, which corresponded to 97.57 ± 0.3% of theoretical density. The highest microhardness of the nanocrystalline bulk alloy reached about 872.5 MPa, which is about three times higher than that of the coarse-grained AZ31.     

Microstructural and mechanical properties of Al-Mg/Al2O3 nanocomposite prepared by mechanical alloying

The effect of milling time on the microstructure and mechanical properties of Al and Al-10 wt.% Mg matrix nanocomposites reinforced with 5 wt.% Al₂O₃ during mechanical alloying was investigated. Steady-state situation was occurred in Al-10Mg/5Al₂O₃ nanocomposite after 20 h, due to solution of Mg into Al matrix, while the situation was not observed in Al/5Al₂O₃ nanocomposite at the same time. For the binary Al-Mg matrix, after 10 h, the predominant phase was an Al-Mg solid solution with an average crystallite size 34 nm. Up to 10 h, the lattice strain increased to about 0.4 and 0.66% for Al and Al-Mg matrix, respectively. The increasing of lattice parameter due to dissolution of Mg atom into Al lattice during milling was significant. By milling for 10 h the dramatic increase in microhardness (155 HV) for Al-Mg matrix nanocomposite was caused by grain refinement and solid solution formation. From 10 to 20 h, slower rate of increasing in microhardness may be attributed to the completion of alloying process, and dynamic and static recovery of powders.     

Multi-phase nanocrystalline Al alloy with superior strength and modulus at elevated temperatures

A multiphase nanocrystalline Al₉₃Fe₃Cr₂Ti₂ alloy containing 30 vol% intermetallic particles was prepared via mechanical alloying, followed by hot extrusion. Systematic compressive tests and modulus measurements were performed as a function of temperature and strain rate. High strengths and moduli at both ambient and elevated temperatures were demonstrated. The results clearly indicated that the multiphase nanocrystalline Al₉₃Fe₃Cr₂Ti₂ alloy has great potential for structural applications. Furthermore, the strength of the multiphase nanocrystalline Al alloy at both room and elevated temperatures increased with the decrease in the grain size, suggesting that diffusional creep is suppressed in this alloy, even though the grain size of the alloy is below 100 nm. This paper was presented at the International Symposium on Manufacturing, Properties, and Application of Nanocrystalline Materials sponsored by the ASM International Nanotechnology Task Force and TMS Powder Materials Committee, October 18–20, 2004, Columbus, OH.     

Mechanical synthesis and rapid consolidation of a nanocrystalline 3.3Fe0.6Cr0.3Al0.1-Al2O3 composite by high frequency induction heating

Nanopowders of 3.3Fe_0.6Cr_0.3Al_0.1 and Al₂O₃ were synthesized from Fe₂O₃, Cr, and Al powders by high-energy ball milling. A high density nanocrystalline 3.3Fe_0.6Cr_0.3Al_0.1-Al₂O₃ composite was consolidated by a high frequency induction heated sintering (HFIHS) method within 3 min from mechanically synthesized powders of Al₂O₃ and 3.3Fe_0.6Cr_0.3Al_0.1. The average grain sizes of Al₂O₃ and 3.3Fe_0.6Cr_0.3Al_0.1 were 84 and 32 nm, respectively.     

Synthesis behavior of nanocrystalline Al-Al2O3 composite during low time mechanical milling process

In this work, four different volume fractions of Al₂O₃ (10, 20, 30 and 40 vol.%) were mixed with the fine Al powder and the powder blends were milled for 5 h. Scanning electron microscopy analysis, particle size analysis and bulk density measurements were used to investigate the morphological changes and achieving the steady state conditions. The results showed that increasing the Al₂O₃ content can provide the steady state particle size in 5 h milling process. It was found that increasing the volume fraction of Al₂O₃ leads to increasing the uniformity of Al₂O₃. Standard deviations of microhardness measurements confirmed this result. The XRD pattern and XRF investigations depicted that increasing the Al₂O₃ content causes an increase in the crystal defects, micro-strain and Fe contamination during 5 h milling process of nanocrystalline composite powders while the grain size is decreased. To investigate the effect of milling time, Al-30 vol.% Al₂O₃ (which achieved steady state during 5 h milling process) was milled for 1-4 h. The results depicted that the milling time lower than 5 h, do not achieve to steady state conditions.     

Transport mechanism in a ceramic system: LiCo3/5Fe1/5Cu1/5VO4

The electrical impedance and modulus properties of a LiCo_3/5Fe_1/5Cu_1/5VO₄ ceramic system were measured by impedance spectroscopy method in the frequency range 10²-10⁶ Hz and temperature range 22-250 °C. X-ray diffraction study reveals formation of the compound in a cubic crystal system with lattice parameters a = 8.2756 (3) Å. Field emission scanning electron microscopy is used to investigate the grain morphology of the material. Nyquist plots confirm the existence of bulk and grain boundary effects at 22 °C ≤ T ≤ 200 °C, and bulk, grain boundary and polarization effects at T ≥ 225 °C. Electrical modulus study indicates a non-Debye behavior of the material. A detailed study of bulk conductivity shows electric conduction in the material as a thermally activated process.     

Perpendicular magnetic anisotropy in 70 nm CoFe2O4 thin films fabricated on SiO2/Si(1 0 0) by the sol-gel method

Cobalt ferrite CoFe₂O₄ films were fabricated on SiO₂/Si(1 0 0) by the sol-gel method. Films crystallized at/above 600 °C are stoichiometric as expected. With increase of the annealing temperature from 600 °C to 750 °C, the columnar grain size of CoFe₂O₄ film increases from 13 nm to 50 nm, resulting in surface roughness increasing from 0.46 nm to 2.55 nm. Magnetic hysteresis loops in both in-plane and out-of-plane directions, at different annealing temperatures, indicate that the films annealed at 750 °C exhibit obvious perpendicular magnetic anisotropy. Simultaneously, with the annealing temperature increasing from 600 °C to 750 °C, the out of plane coercivity increases from 1 kOe to 2.4 kOe and the corresponding saturation magnetization increases from 200 emu/cm³ to 283 emu/cm³. In addition, all crystallized films exhibit cluster-like structured magnetic domains.     

The effects of heat treatments on hardness and wear resistance in Ni-W alloy coatings

The relationship of processing parameters, microstructure, and mechanical responses of the electrodeposited nickel-tungsten alloys exposed to elevated temperatures in the range 700-1100 °C are investigated. Reverse pulse electrodeposition technique is employed to control the tungsten content and nanocrystalline grain size of the deposits. The application of heat treatment at 700 °C on the alloy with high tungsten content (22 at.%) and small grain size (3 nm) gives hardness enhancement and a small decrease in wear resistance. Prolonging annealing duration and increasing annealing temperature promote more grain growth and reductions of both hardness and wear resistance, despite the formations of secondary phases. For alloys with lower tungsten contents (6% and 13%) and larger grain sizes (13 and 56 nm), higher degrees of grain growth coupled with monotonic decline of hardness are observed. The study indicates that the electrodeposited nickel-tungsten alloys with a high tungsten content potentially serve as strong candidates for high temperature applications.     

Effect of air annealing on mechanical properties and structure of amorphous B4C films

Amorphous B₄C films were prepared by magnetron sputtering of the hot-pressed B₄C target in different regimes. Hardness, intrinsic stress and film structure were investigated in dependence on the annealing temperature in air.Changes in the film structure and composition were investigated by Raman spectroscopy, confocal microscopy, and electron probe microanalysis. It has been shown that an annealing at 500 °C for 1 h leads to stress reduction, slight thickness decrease and increase of film hardness. However already at 600 °C the film oxidation proceeds very intensively with formation of the phases of boron oxide and amorphous carbon in the surface layer. The thickness of the film decreases quickly.The film oxidation is accompanied by formation of numerous carbon hillocks and redistribution of film material after annealing in furnace at 500 and especially 600 °C. The oxidation of a-B₄C films as well as of the crystalline bulk samples starts in some locations and has clearly pronounced heterogeneous character that indicates heterogeneous structure of amorphous films as well as of bulk crystalline samples.Annealing in air for a long period shifts down the onset of formation of hillocks to 400 °C and changes in film morphology to 300 °C. Thus the upper temperature limit for application of a-B₄C films in air depends also on the exposure time at the operation temperature.     

A study on the microstructure of D023 Al3Zr and L12 (Al+12.5 at.% Cu)3Zr intermetallic compounds synthesized by PBM and SPS

The spark plasma sintering (SPS) of L1₂ phase Al₃Zr and (Al+12.5 at.% Cu)₃Zr powders with a nanocrystalline microstructure has been studied to produce bulk intermetallic compounds which maintain metastable structures such as L1₂ structure and nanocrystalline microstructure. The powders were prepared by 10 h planetary ball milling (PBM). Full-density L1₂ (Al+12.5 at.% Cu)₃Zr intermetallic compounds were obtained by SPS for 0 min at 600 °C. The specimens prepared with a longer holding time than 0 min at 600 °C or a higher temperature than 600 °C had local melting areas where micro-cracks were found. They had a lower relative density than the specimen SPS sintered at 600 °C for 0 min. The smallest grain size was obtained in the specimen prepared at 600 °C for 0 min, which was 20–30 nm as confirmed by TEM observation. This was the smallest grain size ever reported in the trialuminide specimens processed by various consolidations of nanocrystalline powders. Accordingly, the highest micro-hardness, 989.5 H_V, was obtained in the specimen and this value was three times higher than those of the specimens with micro grain sizes. Full density Al₃Zr intermetallics were prepared by SPS at 700 °C for 0 min. However, their crystal structure was D0₂₃ and micro-hardness was 778.1 H_V. By using SPS, the sintering time can be reduced within 10 min. It was thought that the decrease in sintering temperature for the PBM Al₃Zr and (Al+12.5 at.% Cu)₃Zr powders by 200–300 °C compared with the conventional sintering temperature resulted in the refinement of microstructure to the nano-size level.     

MA-PAS和MA-HP烧结制备的Fe_3Al金属间化合物的组织和力学性能

以机械合金化Fe-28%Al（摩尔分数）合金粉末为原料,分别采用等离子活化烧结（PAS）和热压烧结（HP）方法制备致密度高达99%的Fe3Al金属间化合物。XRD和TEM测试结果表明：PAS烧结试样保留了机械合金化粉末的A2无序结构,并呈现出亚微米晶粒区域（〉1μm）和纳米晶粒区域（〈500nm）双峰分布的特征,而HP烧结试样为部分D03有序结构,晶粒尺寸在1～2μm的范围内。压缩试验表明：在室温至800℃的条件下,采用两种方法烧结的Fe3Al金属间化合物具有近似的压缩强度,虽然当温度超过400℃后压缩屈服强度均急剧下降,但在800℃时其压缩屈服强度仍高达100MPa,远高于铸造态Fe3Al金属间化合物。相比于HP烧结和铸造态Fe3Al金属间化合物,PAS烧结Fe3Al金属间化合物表现出优异的室温塑性,其室温压缩工程应变为20%。组织结构分析和力学性能测试结果表明,超细晶无序组织有利于Fe3Al金属间化合物室温塑性和高温强度的同时增强。     

Ultrasonic-assisted in situ synthesis and characterization of superparamagnetic Fe3O4 nanoparticles

Superparamagnetic Fe₃O₄ nanoparticles were synthesized via a modified coprecipitation method, and were characterized with X-ray diffraction (XRD), vibrating sample magnetometer (VSM), Zeta potential and FT-IR, respectively. The influences of different kinds of surfactants (sodium dodecyl benzene sulfonate, polyethyleneglycol, oleic acid and dextran), temperatures and pH values on the grain size and properties were also investigated. In this method, Fe³⁺ was used as the only Fe source and partially reduced to Fe²⁺ by the reducing agent with precise content. The following reaction between Fe³⁺, Fe²⁺ and hydroxide radical brought pure Fe₃O₄ nanoparticles. The tiny fresh nanoparticles were coated in situ with surfactant under the action of sonication. Comparing with uncoated sample, the mean grain size and saturation magnetization of coated Fe₃O₄ nanoparticles decrease from 18.4 nm to 5.9-9.0 nm, and from 63.89 emu g⁻¹ to 52-58 emu g⁻¹ respectively. When oleic was used as the surfactant, the mean grain size of Fe₃O₄ nanoparticles firstly decreases with the increase of reaction temperature, but when the temperature is exceed to 80 °C, the continuous increase of temperature resulted in larger nanoparticles. the grain size decreases gradually with the increasing of pH values, and it remains unchanged when the PH value is up to 11. The saturation magnetization of as-prepared Fe₃O₄ nanoparticles always decreases with the fall of grain size.     

Phase transformations in face centered cubic (Al0.32Cr0.68)2O3 thin films

Face centered cubic (Al_0.32Cr_0.68)₂O₃ thin films have been annealed in the temperature range of 500–1000 °C during 2–8 h. The fcc structure of the film remains intact when annealed at temperatures up to 700 °C for 8 h. X-ray diffraction and transmission electron microscopy show the onset of phase transformation to corundum phase alloys in the sample annealed at 900 °C for 2 h, where annealing at 1000 °C for 2 h results in complete phase transformation to α-(Al_0.32Cr_0.68)₂O₃. In-plane and out-of-plane line scans performed in EDX TEM and θ/2θ XRD patterns did not show any phase separation into α-Cr₂O₃ and Al₂O₃ prior and after the annealing. The apparent activation energy of this process is 380–480 kJ/mol as determined by the Johnson–Mehl–Avrami model.