Structure of mechanically alloyed Ti-Al-Nb powders

Ti-Al-Nb ternary powder mixtures containing 24Al-11Nb, 25Al-25Nb, 37.5Al-12.5Nb, and 28.5Al-23.9Nb (at. pct) were mechanically alloyed in a SPEX 8000 mixer mill using a ball-to-powder weight ratio of 10:1. The structural evolution in these alloys was investigated by X-ray diffraction and transmission electron microscopy techniques. A solid solution of Al and Nb in Ti was formed at an early stage of milling, followed by the B2/body-centered cubic (bec) and amorphous phases at longer milling times. The stability of these phases and their transformation to other phases have been investigated by heat treating these powders at different temperatures. The B2/bcc phase transformed into an orthorhombic (O-Ti₂AlNb) or a mixture of the orthorhombic (O) and hexagonal close-packed (α₂-Ti₃Al) phases, the proportion of phases being dependent on the powder composition. Milling beyond the amorphous phase formation resulted in the formation of an fee phase in all the powders, which appears to be TiN, formed as a result of contamination of the powder. Formerly Graduate Student, University of Idaho     

Diary

Abstract

The addition of amorphous Fe–Si–B particles to Fe powder increases the shrinkage of sintered components resulting in higher densification rates. Consequently, several research groups worldwide have studied the properties of such systems in an attempt to produce superior structural alloys. In the present work, Fe₇₅Si₁₀B₁₅ ribbons obtained by melt spinning were milled in a high energy Spex mill for times varying from 2 to 32 h. The resulting powders were characterised by differential thermal analysis and X-ray diffraction. The results showed that the amorphous characteristics of the ribbons persisted after the milling process. Next, samples consisting of a mixture of Fe powder and 4 wt-% milled amorphous phase were uniaxially pressed and sintered following a series of thermal cycles. High temperature microstructures were obtained for compacts subjected to rapid cooling from the sintering temperature. The results of scanning electron microscopy and energy dispersive spectroscopy revealed substantial precipitation of fine Fe₂B particles before α → γ allotropic transformation. In addition, an oxide phase was observed in the interface between Fe and the additive particles. Preliminary analysis suggested that the oxide particles can be easily reduced by adding small amounts of carbon to the system. PM/0765     

Microstructures and Properties of Nanocrystalline NiFe Alloy With and Without Particulate TiC Reinforcement by Mechanical Alloying

In the current study, Ni₅₀Fe₅₀ alloy powders were prepared using a high-energy planetary ball mill. The effects of TiC addition (0, 5, 10, 20, and 30 wt pct) and milling time on the sequence of alloy formation, the microstructure, and microhardness of the product were studied. The structure of solid solution phase, the lattice parameter, lattice strain, and grain size were identified by X-ray diffraction analysis. The correlation between the apparent densities and the milling time is explained by the morphologic evolution of the powder particles occurring during the high-energy milling process. The powder morphology was examined using scanning electron microscopy. It was found that FCC γ (Fe–Ni) solid solution was formed after 10 hours of milling, and this time was reduced to 7 hours when TiC was added. Therefore, brittle particles (TiC) accelerate the milling process by increasing crystal defects leading to a shorter diffusion path. Observations of polished cross section showed uniform distribution of the reinforcement particles. The apparent density increases with the increasing TiC content. It was also found that the higher TiC amount leads to larger lattice parameter, higher internal strain, and lower grain size of the alloy.     

Structural evolution in mechanically alloyed Al-Fe powders

The structural evolution in mechanically alloyed binary aluminum-iron powder mixtures containing 1, 4, 7.3, 10.7, and 25 at. pct Fe was investigated using X-ray diffraction (XRD) and electron microscopic techniques. The constitution (number and identity of phases present), microstructure (crystal size, particle size), and transformation behavior of the powders on annealing were studied. The solid solubility of Fe in Al has been extended up to at least 4.5 at. pct, which is close to that observed using rapid solidification (RS) (4.4 at. pct), compared with the equilibrium value of 0.025 at. pct Fe at room temperature. Nanometer-sized grains were observed in as-milled crystalline powders in all compositions. Increasing the ball-to-powder weight ratio (BPR) resulted in a faster rate of decrease of crystal size. A fully amorphous phase was obtained in the Al-25 at. pct Fe composition, and a mixed amorphous phase plus solid solution of Fe in Al was developed in the Al-10.7 at. pct Fe alloy, agreeing well with the predictions made using the semiempirical Miedema model. Heat treatment of the mechanically alloyed powders containing the supersaturated solid solution or the amorphous phase resulted in the formation of the Al₃Fe intermetallic in all but the Al-25 at. pct Fe powders. In the Al-25 at. pct Fe powder, formation of nanocrystalline Al₅Fe₂ was observed directly by milling. Electron microscope studies of the shock-consolidated mechanically alloyed Al-10.7 and 25 at. pct Fe powders indicated that nanometer-sized grains were retained after compaction.     

机械合金化制备Fe-Co系非晶合金

在高纯氩气保护下采用高能球磨法对原子组成为Fe44Co44Zr3.5Nb3.5B4Cu1的混合粉末进行机械合金化(MA)实验,成功地制取了非晶合金粉末.利用X射线衍射(XRD)、扫描电镜(SEM)、差热分析(DTA)对其进行测试,结果表明:Fe-Co系的混合粉末在MA过程中,通过原子之间的相互固溶、扩散可形成非晶态.此非晶合金的形成是晶粒细化、球磨过程中的缺陷、应力和致密堆垛结构等多种因素综合作用的结果,这与机械合金化的合成机理之一的扩散型机制相吻合.用非晶化的热力学条件判据和动力学条件判据对此合金进行计算,其结果也表明此合金已非晶化.     

On selection of milling atmosphere for production of Al–10%Ti powders

Abstract

A mixture of aluminium and 10 wt-% titanium powders was attrition milled for 10 h under air, nitrogen and vacuum atmospheres; pure aluminium powders were also prepared in a like manner. Particle size distribution, morphology and microstructure of the powders were studied by laser diffraction, scanning electron microscopy (SEM) and X-ray diffraction (XRD); special attention was paid to the influence of the milling atmosphere. There were differences in powder particle size obtained from pure Al powders that were not observed for Ti containing powders, however the same homogeneous morphology and microstructure was attained for the different milling atmospheres. The effect of milled powder annealing on microstructure was studied by differential scanning calorimetry (DSC) and XRD. New phases and their crystallite size were characterised as a function of annealing temperature, milling atmosphere, and powder microhardness. In short, the studied milling atmospheres for the production of Al–10%Ti powders do not affect the properties of the obtained powders, and in general, low cost atmospheres could be used.     

Phase Evolution and Mechanical Properties of Nano-TiO2 Dispersed Zr-Based Alloys by Mechanical Alloying and Conventional Sintering

The present study deals with the synthesis of 1.0 to 2.0 wt pct nano-TiO₂ dispersed Zr-based alloy with nominal compositions 45.0Zr-30.0Fe-20.0Ni-5.0Mo (alloy A), 44.0Zr-30.0 Fe-20.0Ni-5.0Mo-1.0TiO₂ (alloy B), 44.0Zr-30.0Fe-20.0Ni-4.5Mo-1.5TiO₂ (alloy C), and 44.0Zr-30.0Fe-20.0Ni-4.0Mo-2.0TiO₂ (alloy D) by mechanical alloying and consolidation of the milled powders using 1 GPa uniaxial pressure for 5 minutes and conventional sintering at 1673 K (1400 °C). The microstructural and phase evolution during each stage of milling and the consolidated products were studied by X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM), and energy-dispersive spectroscopy. The particle size of the milled powder was also analyzed at systemic intervals during milling, and it showed a rapid decrease in particle size in the initial hours of milling. XRD analysis showed a fine crystallite size of 10 to 20 nm after 20 hours of milling and was confirmed by TEM. The recrystallization behavior of the milled powder was studied by differential scanning calorimetry. The hardness of the sintered Zr-based alloys was recorded in the range of 5.1 to 7.0 GPa, which is much higher than that of similar alloys, developed via the melting casting route.     

Compaction and characterization of mechanically alloyed nanocrystalline titanium aluminides

Blended elemental (BE) Ti-24 at. pct Al-11 at. pct Nb (Ti-24-11) and Ti-55 at. pct Al (Ti-55) powders and prealloyed (PA) Ti-24-11 powders were mechanically alloyed in a SPEX mill or an attritor. After SPEX milling for 10 hours, the BE Ti-24-11 powder contained the B2/bcc phase, while the BE Ti-55 powder showed the presence of an amorphous phase. The PA Ti-24-11 powder containing the B2 phase showed a decrease of crystal size on milling. These powders were consolidated by hot isostatic pressing (“hipping”), Ceracon process, and dynamic methods. On compaction, the B2/bcc phase in the Ti-24-11 sample transformed to a mixture of the B2 and orthorhombic (“O”) phases, while the amorphous phase in the Ti-55 powder crystallized to a mixture of the γ-TiAl and α ₂-Ti₃Al phases. The finest grain size in compacted material was obtained in the dynamically consolidated powder, and the grain size in the hot isostatic pressed (“hipped”) powder became larger with the increasing hipping temperature.     

Preparation and thermal stability of Zr-Ti-Al-Ni-Cu amorphous powders by mechanical alloying technique

This study examined the amorphization feasibility of Zr_70−x−y Ti _x Al _y Ni₁₀Cu₂₀ alloy powders by the mechanical alloying (MA) technique. According to the results, after 5 to 7 hours of milling, the mechanically alloyed powders were amorphous basically in the ranges of 0 to 12.5 at. pct Ti and 2.5 to 17.5 at. pct Al. These ranges are larger than those of bulk amorphous alloys prepared by a squeeze mold casting technique. Most of the amorphous mechanically alloyed powders exhibited a wide supercooled liquid region of more than 60 K before crystallization. The glass-transition and crystallization temperatures of mechanically alloyed samples were different from those prepared by squeeze casting. It is suspected that different thermal properties arise from the introduction of impurities during the MA process. The amorphization behavior of Zr₅₀Ti_7.5Al_12.5Ni₁₀Cu₂₀ was examined in detail. The X-ray diffraction and extended X-ray absorption fine structure (EXAFS) results show the fully amorphous powders formed after 5 hours of milling. A kinetically modified thermodynamic phase transformation process was observed for the glass-transition behavior in the Zr₅₀Ti_7.5Al_12.5Ni₁₀Cu₂₀ amorphous powder.     

Fabrication of Al2O3/(ZrB2 + TiB2) Composite Using MACS and Microwaves

Because of the excellent thermal and mechanical properties of engineering ceramics, they have been used as structural materials or composite matrixes and reinforcements in recent years. Alumina, titanium diboride, and zirconium diboride have found important uses in the past two decades. In this study, Al₂O₃/(ZrB₂ + TiB₂) ceramic composite powders were fabricated in situ and mechanical activation by milling was used to assist combustion synthesis (CS). A mixture of Al, ZrO₂, TiO₂, and B₂O₃ powders were used as raw materials. Mechanical activation was done using ball milling of different durations. Afterward, combustion was initiated using microwaves on the activated mixtures. X-ray diffraction (XRD) and scanning electron microscopy were used to investigate the purity and microstructure of the products. XRD analysis of the samples in the final stages of the process revealed that Al₂O₃/(ZrB₂ + TiB₂) composite powder was successfully fabricated using mechanical activation and CS, but that the CS reaction did not occur in unmilled samples. It was shown that increasing milling time from 3 to 10 hours increased purity and homogeneity of the products to the point that no noticeable impurity existed in the samples milled for 10 hours.     

Phase transformation,structural evolution and mechanical property of nanostructured FeAl as a result of mechanical alloying

Objective of the work was to synthesize nanostructured FeAl alloy powder by mechanical alloying (MEA). The work concentrated on synthesis, characterization, structural and mechanical properties of the alloy. Nanostructured FeAl intermetallics were prepared directly by MEA in a high energy rate ball mill. Milling was performed under toluene solution to avoid contamination from the milling media and atmosphere. Mixtures of elemental Fe and Al were progressively transformed into a partially disordered solid solution with an average composition of Fe—50 at % Al. Phase transformation, structural changes, morphology, particle size measurement and chemical composition during MEA were investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Energy dispersive X-ray spectroscopy (EDS) respectively. Vickers micro hardness (VMH) indentation tests were performed on the powders. XRD and SEM studies revealed the alloying of elemental powders as well as transition to nanostructured alloy, crystallite size of 18 nm was obtained after 28 hours of milling. Expansion/contraction in lattice parameter accompanied by reduction in crystallite size occurs during transition to nanostructured alloy. Longer milling duration introduces ordering in the alloyed powders as proved by the presence of superlattice reflection. Elemental and alloyed phase coexist while hardness increased during MEA.     

Structure and Properties of Dysprosium Titanate Powder Produced by the Mechanochemical Method

The structure and main physicochemical properties of dysprosium titanate powders prepared by mechanochemical synthesis from the low-temperature modification of titanium oxide and modification of dysprosium oxide are investigated applying X-ray phase analysis (XPA), scanning electron microscopy, Raman spectroscopy (Raman spectra), transmission electron microscopy, and chemical analysis. It is established based on XPA that the initial oxides completely transform into X-ray amorphous dysprosium titanate (Dy₂TiO₅) during the mechanochemical treatment of a mixture for 30–60 min. A microelectron diffraction pattern of Dy₂TiO₅ powders prepared by mechanosynthesis has a ring structure characteristic of the X-ray amorphous phase with a certain amount of inclusions of a crystalline phase. The dysprosium titanate powder fabricated by induction melting possesses the regular cubic crystalline lattice with a parameter of 3.4 Å.     

Morphological and calorimetric studies on the

Amorphous Al₅₀Zr₅₀ alloy powders have been prepared by rod-milling technique using mechanical alloying (MA) method. The amorphization and crystallization processes of the alloyed powders were followed by optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), differential thermal analysis (DTA), and differential scanning calorimetry (DSC). The results have shown that the formation of amorphous Al₅₀Zr₅₀ alloy powders occurs through three stages, agglomeration, disintegration, and homogenization. At the disintegration stage, the alloyed powders contain many fine layers of Al and Zr. An amorphous phase has been formed at about 880 K as a result of heating these layered particles in a thermal analyzer. The crystalline-to-amorphous transformation at this stage of milling is attributed to a thermally assisted solid-state amorphizing reaction. The present study corroborates the similarity of the amorphization process through the MA with the solid-state interdiffusion reaction in multilayered thin films. The amorphization temperature, T_a, and the activation energy of amorphization, E_a, are 675 and 156 kJ/mol, respectively. In addition, the enthalpy change of amorphization, ΔH_a, was evaluated to be -3.5 kJ/mol. On the other hand, the crystallization temperature, T_x, and enthalpy change of crystallization, ΔH_x, were 1000 K and −68 kJ/mol, respectively.     

Structure and magnetic properties of nanocrystalline Ni0·64Zn0·36Fe2O4 powders prepared by ball milling

Abstract

In this study, nanocrystalline Ni_0·64Zn_0·36Fe₂O₄ powders were prepared using a planetary ball mill. The evolution of the microstructure and magnetic properties during the milling were studied by X-ray diffraction technique, scanning electron microscopy, transmission electron microscopy and vibrating sample magnetometre. It is revealed from the results of the phase analysis that nanocrystalline Ni_0·64Zn_0·36Fe₂O₄ ferrite with average crystallite size of 6·18 nm and non-uniform lattice strain of 0·33% has been formed after 60 h of milling time. A progressive increase of saturation magnetisation and a dramatic decrease in coercivity were also observed with increasing milling time.     

Thermally assisted and mechanically driven solid-state reactions for formation of amorphous AI33Ta67 alloy powders

The rod milling technique using the mechanical alloying (MA) process has been employed for preparing amorphous Al₃₃Ta₆₇ alloy starting from elemental Al and Ta powders. X-ray diffraction (XRD), differential thermal analysis (DTA), differential scanning calorimetry (DSC), optical microscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM) are utilized to follow the progress of amorphization. The results show that during the first few kiloseconds of MA time, layered composite particles of Al and Ta are intermixed and form an amorphous phase upon heating to 685 K by DTA. This process is called thermally assisted solid-state amorphization (TASSA). During the early stage of milling, the number of layers of the composite particles increases. This leads to an increase in the heat formation of amorphous Al₃₃Ta₆₇ alloyvia the TASSA process, ΔH _TASSA ^a . After 360 ks (100 h) of the MA time, all Al atoms emigrate to Ta lattices to form a solid solution phase and the powder particles have no more layered structure. At this stage of milling, the value of ΔH _TASSA ^a becomes zero. This solid solution phase is not stable against the shear forces that are generated by the rods and transforms completely to an amorphous phase upon milling for 720 ks (200 hours). This phase transformation is attributed to the accumulation of several lattice imperfections, such as point and lattice defects, which raise the free energy from the more stable phase (solid solution) to a less stable phase (amorphous). After 1440 ks (400 hours) of MA time, a homogeneous amorphous phase is formed. The amorphization process in this case is attributed to a mechanical driven solid-state amorphization (MDSSA). The heat of formation of the amorphous phase formedvia the MDSSA process, ΔH _MDSSA ^a , has been calculated. Moreover, the crystallization characteristics indexed by the crystallization temperature, and the enthalphy of crystallization, of the amorphous phases formed by TASSA and MDSSA processes are investigated as a function of MA time. The role of amorphizationvia each process has been discussed. Formerly lecturer of Materials Science, Department of Mining and Petroleum Engineering, Faculty of Engineering, AI-Azhar University, Nasr City 11884, Cairo, Egypt     

Combustion synthesis of Fe–Al/TiC composite powders and effect of Al content on its characteristics

Abstract

In this work, combustion synthesis of ferrotitanium–Al–C powder mixtures with different compositions was carried out to synthesise Fe–Al/TiC composites. Differential thermal analysis was performed on the precursor powder from ambient temperature to 1673 K at a heating rate of 30 K min^?1. Phase development and structural changes were investigated by X-ray diffraction technique and scanning electron microscopy. The results showed that no trace of TiAl_x (x?=?1, 3) was formed in all samples, and the reaction of (Ti–Fe)–Al–C system took place in the following two steps: first, molten Al and Fe reacted exothermically to form Fe–Al intermetallic compound. Second, the produced heat melted the ferrotitanium with lower Fe content and resulted in a liquid containing Ti, Fe, Al and C. TiC formed in all samples, but depending on the Al content, different phases containing FeAl₂, FeAl, Fe₃Al, Fe₃AlC_x and α-Fe formed as phases of matrix. The mixture with the lower Al content gave out a higher combustion temperature.     

合金元素对机械合金化和放电等离子烧结Ti-Nb基合金显微组织的影响

β-Ti型结构的钛基材料在生物材料领域具有广泛的应用前景。本文采用机械合金化法和放电等离子烧结制备β-Ti型Ti-Nb基合金,研究不同Nb,Fe含量对合金显微组织及力学性能的影响。利用扫描电镜(SEM)、X射线衍射仪(XRD)和透射电镜(TEM)等手段分析合金的显微组织变化情况。结果表明:机械合金化过程中,粉末的平均粒度减小,当球磨时间超过60 h时粉末易发生团聚。当球磨转速为300 r/min,球料比为12:1,Ti和Nb的质量分数分别为64%和24%时,球磨100 h后制备的粉体材料中具有一定体积的非晶相。该粉末在1 000℃下通过放电等离子烧结(SPS)制备具有均匀细小的球状晶粒组织的Ti-Nb合金,其强度、伸长率和弹性模量分别为2 180MPa,6.7%和55 GPa。通过控制Nb,Fe的含量,可以促进β-Ti相形成,获得高强度和低杨氏模量的Ti-Nb合金。     

Combustion synthesis of Fe3Al/TiC composite powders

Abstract

A mixture of (FeTi₂+C)+10 at-%Al based on stoichiometry of Fe₃Al+TiC was used for a combustion front quenching test. The microstructural evolution during combustion synthesis was analysed by scanning electron microscopy and energy dispersive spectrometry. The phase constituents of the product were evaluated by X-ray diffraction. At first, Al powders were melted at 933 K and surrounded FeTi₂ particles and carbon powders. When the temperature increased to 1358 K, FeTi₂ melted, and Al and C dissolved in Fe and Ti. Then, solid–liquid and liquid–liquid reactions took place, and TiC and Fe₃Al formed. At least at 1723 K, the iron aluminide phase surrounded large TiC particles. Because of formation of TiC_0·95, a small amount of carbon remained in matrix and reacted with Fe₃Al and formed Fe₃AlC. Based on these results, the mechanism of the Fe₃Al–TiC combustion synthesis could be described with a ternary solution precipitation mechanism.     

Synthesis and characterisation of quasicrystalline Al based composites

Abstract

Al matrix composites reinforced by Al–Cu–Fe quasicrystalline (QC) phase particles were produced from a mixture of Al and QC powders using electrical current heating and conventional sintering. A combination of X-ray diffractrometry, transmission and scanning electron microscopy was used to characterise the microstructure of consolidated specimens. The metallic bonding of the Al matrix and particles was improved by higher temperature sintering or electrical current heating. However, the dissolution of QC particles into the Al matrix was inevitable during heating and resulted in the formation of ω and/or β phases. The dissolution of QC particles was effectively reduced using prealloyed Al powder containing 2 at.-%Cu. This had led to an increase in microhardness from 96 to 139 HV for specimens using pure Al to prealloyed Al powders. A homogeneous distribution of QC particles within the Al matrix could be achieved by mechanical milling followed by consolidation.     

球磨参数对Fe_(73.5)Cu_1Nb_3Si_(13.5)B_9产物微观结构的影响

研究了机械合金化法制备Fe_(73.5)Cu_1Nb_3Si_(13.5)B_9非晶先驱体的可行性,测试了不同球磨参数对Fe_(73.5)Cu_1Nb_3Si_(13.5)B_9球磨产物微观结构的影响。试验结果表明:转速、球磨时间、球磨方式、球料比和原料对产物的微观结构有明显的影响。高转速、连续球磨更有利于生成Fe_(73.5)Cu_1Nb_3Si_(13.5)B_9非晶相;使用Fe Nb粉和Fe B粉分别代替Nb粉和B粉不利于非晶相的生成;延长球磨时间不一定对非晶化有利,还有可能引入杂质;大的球料比更有利于非晶相的生成。