Synthesis and Characterization of Nanocrystalline Ni-Ti and Ni-Cr Powders by Mechanical Alloying

Nanocrystalline powders in the Ni-Ti and Ni-Cr systems were prepared by mechanical alloying (MA) of elemental crystalline powders in an inert atmosphere. The microstructure of the mechanically alloyed powders were characterized by XRD and TEM. The ball-milling process results in a drastic decrease of the crystallite size to the nanometer scale. X-ray diffraction analysis reveals that in the Ni-Cr system, no diffraction peaks from NiCr compound were observed even after 20 h of ball milling; while the lattice parameter of Ni increased with the milling time. In the Ni-Ti system, amorphous alloy was formed. Crystalline intermetallic compounds were obtained by post heat treatment of the amorphous alloy.The crystallization temperature of the amorphous NiTi alloy was obtained be DSC measurement.     

Changes in the oxygen content,morphology, and microstructure of Mo-10Nb composite powders during mechanical alloying

The prefabrication of Mo-Nb composite powders is an effective way of improving the homogeneity of Mo-10Nb targets, which have broad application prospects in the photoelectric sensor industry. However, this aspect has been rarely addressed so far. Therefore, we prepared Mo-10Nb composite powders by mechanical alloying (MA), and investigated the effects of the experimental parameters such as the milling speed and duration on the particle morphology, size distribution, compositional homogeneity, crystallite size, inner strain, and oxygen content. High-quality Mo-10Nb composite powders with 3-μm spherical particles of narrow size distribution, homogeneous elemental distribution, and nanometric crystalline structure were obtained by implementing optimum MA parameters, viz., a milling speed of 250 rpm and duration of 36 h using an MITR QM-QX-4L omnidirectional ball mill. The mechanically alloyed Mo-10Nb composite powders were prone to oxidation when exposed to air, which led to a sharp increase in the oxygen content to ~5400 ppm. X-ray photoelectron spectroscopic analysis revealed the presence of Nb₂O₅, MoO₂, and MoO₃ on the surface of the Mo-10Nb particle. We believe that this study demonstrates an interesting strategy for the fabrication of high-quality Mo-10Nb targets.     

Mechanical alloying and consolidation of copper-iron-silicon carbide nanocomposites

Mechanical alloying, cold pressing, and sintering were used for synthesizing bulk copper, copper-iron, and copper-iron-silicon carbide nanomaterials. The precipitation of iron during sintering of the supersaturated mechanically alloyed powder significantly enhanced the thermal stability of the nanocomposite against grain growth. Moreover, the hardness of sintered composites was found to increase with increasing milling time, which was attributed to the work-hardening, crystallite refinement, and increasing the relative density (decrease in porosity). Although the addition of silicon carbide did not affect the mean crystallite size of the bulk samples, it effectively increased the hardness of the nanocomposite based on its composite strengthening effect.     

粉末冶金TiVNbTa难熔高熵合金的组织和力学性能

将机械合金化(MA)与放电等离子烧结(SPS)相结合制备了难熔TiVNbTa高熵合金,研究了这种合金的机械合金化过程、相组成和显微组织,以及烧结温度和O、N含量对其力学性能的影响。结果表明:机械合金化后高熵合金粉末为BCC结构,放电等离子烧结成的块体高熵合金由BCC基体和FCC析出相组成,其析出相为TiN+TiC+TiO的复合物。烧结温度为1100℃的高熵合金具有良好的综合力学性能,压缩屈服强度达到1506.3 MPa,塑性应变为33.2%。随着烧结温度的提高,合金发生了从准脆性到塑性再到脆性断裂的转变。O和N含量的提高对高熵合金强度的影响较小,但是使其塑性显著降低。     

Sintering behavior of mechanically alloyed Ti-48Al-2Nb aluminides

Ti-Al intermetallics have been produced using mechanical alloying technique. A composition of Ti-48Al-2Nb at % powders was mechanically alloyed for various durations of 20, 40, 60, 80 and 100 h. At the early stages of milling, a Ti (Al) solid solution is formed, on further milling the formation of amorphous phase occurs. Traces of TiAl and Ti₃Al were formed with major Ti and Al phases after milling at 40 h and beyond. When further milled, phases of intermetallic compounds like TiAl and Ti₃Al were formed after 80 hours of milling and they also found in 100 h milled powders. The powders milled for different durations were sintered at 785°C in vacuum. The mechanically alloyed powders as well as the sintered compacts were characterized by XRD, FESEM and DTA to determine the phases, crystallite size, microstructures and the influence of sintering over mechanical alloying.     

Effect of rotation speed and milling time to attain Nb-10Hf-1Ti alloy powders on morphology and microstructure of Nb-10Hf-1Ti powder

The mechanical alloying process was employed to produce C103 alloy with Nb-10% Hf-1% Ti (wt.%) composition using Nb, Hf and Ti powders. The mechanical alloying process was performed in an argon atmosphere in the chamber and bullets of tungsten carbide with a ball-to-powder weight ratio (BPR) of 20:1 at rotation speed of 200, 300 and 400 rpm for 2, 5 and 8 h. At rotation speeds of 200 and 300 rpm particle size decreased and became more spherical during MA. While increasing milling time at 400 rpm caused agglomeration of particles. XRD results showed that increasing milling time at a constant rotation speed has no considerable effect on reduction of crystallite size, but the lattice strain is strongly affected by it and increased obviously with further rotation speed. The results showed that the optimum milling time and rotation speed to attain Nb-10Hf-1Ti alloy powders with the least amount of contamination and appropriate morphology are 5 h and 300 rpm, respectively.     

Electrocatalytic properties of mechanically alloyed Co-20wt%Ni-10wt%Mo and Co-70wt%Ni-10wt%Mo alloy powders

Mechanically alloyed Co-20wt%Ni-10wt%Mo and Co-70wt%Ni-10wt%Mo (nominal compositions) alloy powders were produced by milling of pure elemental powders. Mechanically alloyed powders were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. MA powder specimens were tested electrollitically in a 30% KOH aqueous solution at 298 K. X-ray diffraction analysis and transmission electron microscopy of milled powders showed the presence of two phases, an fcc solid solution and intermetallic compounds of Ni or Co with Mo. These phases showed a nanometric size. The linear sweep voltammograms confirmed also the presence of two phases in both mechanically alloyed alloy powders. The Co-20wt%Ni-10wt%Mo alloy powders showed the best electrocatalytic activity for hydrogen evolution reaction.     

Synthesis and characterization of Al-Zn/Al2O3 nano-powder composites

Composites consisting of Al-Zn/Al2O3 have been synthesized using high energy mechanical milling. High energy ball milling increases the sintering rate of the composite powder due to increased diffusion rate. Owing to the finer microstructure, the hardness of the sintered composite produced by using the mechanically milled nanocomposite powder is significantly higher than that of the sintered composite produced by using the as-mixed powder. The mean crystallite size of the matrix has been determined to be 27 nm by Scherrer equation using X-ray diffraction data. The powders have been characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and differential thermal analysis (DTA). The effect of high-energy ball milling and subsequent annealing on a mixture of Al and ZnO has also been investigated. DTA result show that the reaction temperature of Al-ZnO decreases with the increase in the ball milling time.     

Nitriding of Fe–18Cr–11Mn powders using mechanical alloying method through aerating nitrogen circularly

Mechanical alloying (MA) method was applied to nitride Fe–18Cr–11Mn stainless steel powders through aerating nitrogen circularly. Both the MA process and increasing nitrogen pressure circularly caused the expansion of nitrogen solubility in Fe. The microstructure of powders was affected by the milling time. The phase transformation of α-Fe to γ-Fe occurred during the MA process. The grain size of powder decreased, while the internal lattice strain increased by increasing the milling time and cycles of aerating nitrogen. The as-milled powder could obtain a fully austenitic structure after sintering and subsequent water quenching. The sintered samples had better density and higher microhardness when the powders milled for more time. The formation mechanism of nitriding of stainless steel powders using MA method in nitrogen was presented.     

高能球磨时间和退火温度对制备TiNi合金粉的影响

为获得高能球磨时间和退火温度对TiNi机械合金粉特性的影响机制,采用X射线衍射(XRD)、扫描电子显微镜(SEM)、X射线能谱仪(EDS)、差示扫描量热法(DSC)等分析方法对TiNi合金粉进行了研究。结果表明,机械合金的相成分随着在氩气保护气氛中的球磨时间和退火温度的不同而发生变化。球磨22h的产物是非晶态TiNi合金、Ti的固溶体、Ni的固溶体,球磨27h的产物是非晶态TiNi合金粉和Ni固溶体相,球磨30h发生了明显的固相反应,生成了TiNi、Ni3Ti、Ti3Ni4等物相;在650℃/5h和1000℃/5h下的退火产物都是Ni3Ti、Ti2Ni、TiNi2、TiNi和TiC,但在上述2个退火温度下TiNi并不是主要物相,其中在650℃退火时TiNi的含量明显更低。     

Synthesis, characterization and annealing of mechanically alloyed nanostructured FeAl powder

Elemental powders of Fe and Al were mechanically alloyed using a high energy rate ball mill. A nanostructure disordered Fe(Al) solid solution was formed at an early stage. After 28 h of milling, it was found that the Fe(Al) solid solution was transformed into an ordered FeAl phase. During the entire ball milling process, the elemental phase co-existed with the alloyed phase. Ball milling was performed under toluene to minimise atmospheric contamination. Ball milled powders were subsequently annealed to induce more ordering. Phase transformation and structural changes during mechanical alloying (MEA) and subsequent annealing were investigated by X-ray diffraction (XRD). Scanning electron microscope (SEM) was employed to examine the morphology of the powders and to measure the powder particle size. Energy dispersive spectroscopy (EDS) was utilised to examine the composition of mechanically alloyed powder particles. XRD and EDS were also employed to examine the atmospheric and milling media contamination. Phase transformation at elevated temperatures was examined by differential scanning calorimeter (DSC). The crystallite size obtained after 28 h of milling time was around 18 nm. Ordering was characterised by small reduction in crystallite size while large reduction was observed during disordering. Micro hardness was influenced by Crystallite size and structural transformation.     

机械合金化合成高临界场Sm0.85Nd0.15FeAsO0.85F0.15超导体（英文）

通过采用机械合金化方法制备的高活性的粉体,可以高度可重复性地制备高质量的铁基超导材料Sm0.85Nd0.15FeAsO0.85F0.15.样品具有高临界温度Tc(约51 K)和高临界场Hc2(达到377 T).由WHH公式确定的Hc2显著高于常规固相方法制备样品的典型值(<200 T).高的临界磁场Hc2与样品微结构有很大关系.机械合金化处理的原始粉体包含大量的晶格畸变缺陷,在快速升温和低温退火制备的小晶粒陶瓷样品中这些缺陷会部分残留,因此形成有效的磁通钉扎,从而提高样品的临界场.     

机械合金化-放电等离子烧结Al2Cu颗粒增强Al基复合材料的制备

以Al粉和Cu粉为原料,采用机械合金化(MA)和放电等离子烧结(SPS)工艺,原位合成了致密的Al₂Cu/Al块体复合材料,着重研究了MA过程中粉末的形貌、尺寸和物相结构的变化以及SPS后复合材料的微观组织和力学性能。结果表明: 在MA过程中,随着MA时间延长,部分Cu原子逐渐固溶于Al原子晶格中,形成均匀过饱和的固溶体Al(Cu);在SPS过程中,Cu从过饱和固溶体中析出并与Al反应形成Al₂Cu颗粒,且弥散分布于Al基体中,形成Al₂Cu/Al复合材料;Al₂Cu/Al复合材料的致密度高达98.7%,室温下的压缩断裂强度为611.3 MPa,延伸率为9.6%,具有良好的力学性能。     

Mechanical Alloying of Ti50Al50 Powders and Their Consolidated Properties

Elemental powder mixtures of 50Ti-50Al (at.%) were mechanically alloyed via various ball milling methods. The microstructural evolution during the milling indicates that the mechanical alloying behavior is strongly affected by milling methods, and horizontal ball milling is most effective for producing homogeneous metastable powders. The mechanically alloyed powders were consolidated by vacuum hot pressing followed by homogeneous annealing. Compression testing results showed that the annealed specimens still retain fine grains and have a good combination of fracture strength and ductility, as compared to cast specimens of the same alloy.     

Comparative study on sintering behavior of Al86Ni6Y4.5Co2La1.5 mechanically alloyed amorphous powder and melt-spun ribbon

In this research work, the sintering characteristics of Al₈₆Ni₆Y_4.5Co₂La_1.5 mechanically alloyed amorphous powders and milled melt spun ribbon have been compared. Mechanically alloyed amorphous powders were synthesized via 200?h high energy ball milling. Melt spun ribbons were synthesized by single roller melt spinning technique and grounded to powder form by ball milling. Mechanically induced partial crystallization occurred in the ribbons during milling. Significantly higher amount of contaminations such as carbon, oxygen and iron were observed in the mechanically alloyed amorphous powders compared to the milled ribbons. Both powders were consolidated via spark plasma sintering. Superior particle bonding was found in the sample consolidated from milled ribbons, ascribed to the lower amount of contamination that could not effectively restrict the viscous flow and diffusion of atoms. Various complex crystalline phases evolved in the sample consolidated from milled ribbon particles due to the presence of crystalline phases in the powders which acted as nucleation sites, whereas the amorphous phase was mostly retained in its counterpart. Vickers microhardness of the consolidated alloys from milled ribbon and mechanically alloyed amorphous powders were 3.60?±?0.13?GPa and 2.53?±?0.09?GPa, respectively. The higher hardness in the former case was attributed to the superior particle bonding and distribution of hard intermetallic phases in the amorphous matrix.     

Ti-Al-Al2O3纳米粉体的机械活化-放电等离子烧结

TiAl基合金是很有发展潜力的高温结构材料,为实现快速高效制备此材料,采用新型的机械活化-放电等离子烧结(MA-SPS)制备纳米材料的有效方法,原位制备Ti-Al金属间化合物Ti-47%Al-10%Al2O3(Al为原子分数,Al2O3为质量分数)材料.介绍了放电等离子烧结这种新兴的纳米固体材料制备技术的特点,结合Ti-Al基合金的具体制备工艺,对MA-SPS的特征予以详细分析研究.通过X射线衍射、扫描电镜、透射电镜等分析,经机械球磨活化后,得到晶粒度小于24 nm的纳米单质元素粉体,为后续原位烧结提供合适的烧结原料.其中添加的Al2O3起到细化晶粒、促进纳米化和机械活化、提高出粉率等作用.纳米粉体在合适的参数下经放电等离子烧结后,可得到致密度达98.7%的(TiAl Ti3Al)理想双相组织,其成分的晶粒度小于91 nm,成为纳米固体材料.     

Formation of W-Re Solid Solution by Mechanical Alloying

Progress of mechanical alloying (MA) during milling of W with Re, in a SPEX Mill was monitored by x-ray diffraction, scanning electron microscopy and transmission electron microscopy. XRD patterns showed continuous decrease in the intensity of Re peaks with increasing MA time. However the Re peaks continued to be present even after 18 ks of milling. 36 kiloseconds of milling showed complete dissolution of Re, as observed by the absence of Re peaks in association with W peak shift in accordance with the dissolution of Re in W. Chemical homogeneity and extensive reduction in particle size of the alloy could be established by microstructural and chemical analysis using SEM and TEM. Isothermal heat treatment of the mechanically alloyed sample at 1700 K for 4 hours did not show any decomposition of the alloy. A similar heat treatment of the blended elemental powder showed the formation of metastable phase formation, possibly at the boundary of dissimilar powder particles. After pressing and sintering of pellets, tests revealed some amount of alloy contamination by iron through milling.     

Microstructure and mechanical properties of ultra-fine grained MoNbTaTiV refractory high-entropy alloy fabricated by spark plasma sintering

The MoNbTaTiV refractory high-entropy alloy(RHEA) with ultra-fine grains and homogeneous microstructure was successfully fabricated by mechanical alloying(MA) and spark plasma sintering(SPS).The microstructural evolutions,mechanical properties and strengthening mechanisms of the alloys were systematically investigated.The nanocrystalline mechanically alloyed powders with simple bodycentered cubic(BCC) phase were obtained after 40 h MA process.Afterward,the powders were sintered using SPS in the temperature range from 1500 ℃ to 1700 ℃.The bulk alloys were consisted of submicron scale BCC matrix and face-centered cubic(FCC) precipitation phases.The bulk alloy sintered at 1600℃ had an average grain size of 0.58 μm and an FCC precipitation phase of 0.18 μm,exhibiting outstanding micro-hardness of 542 HV,compressive yield strength of 2208 MPa,fracture strength of 3238 MPa and acceptable plastic strain of 24.9% at room temperature.The enhanced mechanical properties of the MoNbTaTiV RHEA fabricated by MA and SPS were mainly attributed to the grain boundary strengthening and the interstitial solid solution strengthening.It is expectable that the MA and SPS processes are the promising methods to synthesize ultra-fine grains and homogenous microstructural RHEA with excellent mechanical properties.     

Characterization of Al/SiC Nanocomposite Prepared by Mechanical Alloying Process Using Artificial Neural Network Model

An artificial neural network model was developed for modeling of the effects of mechanical alloying process parameters including milling time, milling speed, and ball-to-powder weight ratio on the crystallite size and lattice strain of the aluminum for Al/SiC nanocomposite powders. A Multilayer Perceptron (MLP) and Radial Basis Function (RBF) networks were used. It was found that MLP network yields better results compared to RBF network with a high correlation coefficients. The neural network model in agreement with other experimental results and theories was shown the variations of the crystallite size and lattice strain of the aluminum against the process parameters.     

Microstructural and mechanical characterisation of ODS ferritic alloys produced by mechanical alloying and spark plasma sintering

Abstract

Powders with nominal composition Fe–14Cr–2W–0·4Ti were mechanically alloyed (MA) with Y₂O₃ in a planetary ball mill at two different rotational speeds. Consolidation of the as milled powders was performed by spark plasma sintering (SPS). As milled powders showed a highly deformed microstructure with elongated nanometre grains and, depending upon the rotational speed, different stages of the nanocluster evolution were observed to be produced. In the case of consolidated materials, grain growth occurred during the SPS process and it was possible to observe the influence of the MA parameters, with larger and more homogeneously distributed grains at the higher rotational speed. Additionally, Ti was observed to be incorporated to the nanoclusters after SPS, indicating a further step in their evolution during consolidation. The mechanical behaviour of the SPS compacts was evaluated by tensile and small punch testing also showing the influence of the MA parameters in the material behaviour.