A study of densification and on factors affecting the density of Ni x –Fe100 − x nanopowders prepared by mechanical alloying and sintered by spark plasma

Mechanical alloying through high-energy ball milling was used in the production of Ni–Fe alloy powders from elemental Ni and Fe powders of average particle size 80 and 25 μm, respectively. High-energy planetary ball milling at room temperature was performed for various time durations ranging between 2 and 100 h. SPS apparatus was used for sintering of powder particles. Density of all specimens was reported and a maximum densification of 99 % was achieved in 50 wt.% Ni–Fe milled for 16 h prior to spark plasma sintering at 1,223 K.     

石英砂超细粉碎的团聚机理与抑制方法的研究

介绍了球磨法粉碎石英砂的原理和粉体颗粒的粒度分布特征,分析了球磨过程中石英粉体颗粒团聚的机理,提出了增加分散剂和分散介质解决球磨过程的团聚问题,并定量地研究了分散剂和分散介质的交互作用关系。粉体颗粒的团聚严重影响检测精度,本文结合超声波技术,研究了石英粉体超声分散方法,确定了最佳超声分散时间。     

Structure studies of ball-milled ZrCuAl, NiTiZrCu and melt-spun ZrNiTiCuAl alloys

ZrNiTiCu and ZrNiTiCuAl alloys were amorphized using either a melt‐spinning or ball‐milling process in a high‐energy planetary mill. The elemental powders were initially blended to the desired composition (in at.%) of Zr, 65; Cu, 27.5; Al, 7.5 and of Ti, 25; Zr, 17; Cu, 29; Ni, 29, respectively. The composition of alloys was chosen to be the same as for the bulk amorphous ZrCuAl and easy glass‐forming ZrNiTiCu alloys. An almost fully amorphous structure was obtained after 80 h of milling in the case of both compositions. Transmission electron microscopy studies of ball‐milled powders revealed the presence of nano‐crystallites [2–5 nm for ZrCuAl and smaller (1–3 nm) for the ZrTiNiCu alloy]. High‐resolution transmission electron microscopy of melt‐spun ZrNiTiCuAl ribbons provided evidence of the amorphous structure.     

Combined FTIR and SEM‐EDS study of Bi2O3 doped ZnO–SnO2 ceramics

The effects of Bi₂O₃ addition on the phase composition, microstructure and optical properties of ZnO–SnO₂ ceramics were investigated. Starting powders of ZnO and SnO₂ were mixed in the molar ratio 2:1. After adding Bi₂O₃ (1.0 mol.%) this mixture was mechanically activated for 10 min in a planetary ball mill, uniaxially pressed and sintered at 1300°C for 2 h. Far‐infrared reflection spectra were measured (100–1000 cm^–1). To investigate the occurred differences in FTIR spectra, the Bi₂O₃‐doped sample was examined more carefully with a Perkin–Elmer FTIR spectrometer (Perkin Elmer, Waltham, MA, USA) connected with a Perkin–Elmer FTIR microscope and itemized points of interest were also studied with SEM‐EDS.     

软金属润滑纳米体研磨制备方法研究

采用行星式球磨机和湿式研磨法，以铅为对象探讨了制备软金属纳米粒子体的工艺方法和研磨机理。研究表明，软金属研磨时，研磨粒子体应力状况的控制非常重要。采用了低转速、小磨球和长时间的特殊研磨工艺，以加入少量表面活性剂的二甲基硅油作为研磨介质，研磨出分散均匀的纳米级软金属颗粒和硅油复合胶体。     

Determining the effect of process parameters on particle size in mechanical milling using the Taguchi method: Measurement and analysis

Micro and nano-particles have been successfully and widely applied in many industrial applications. The mechanical milling process is a popular technique used to produce micro and nano-particles. Therefore, it is very important to improve milling process efficiency and quality by determining the optimal milling parameters. In this study, the effects of the main mechanical milling parameters: milling time, process control agent (PCA), ball to powder ratio (BPR) and milling speed in the planetary ball milling of nanocrystalline Al 2024 powder were optimized by the Taguchi method. Mean particle size (d₅₀) was used to evaluate the effect of process parameters on the mechanical milling process. The orthogonal array experiment is conducted to economically obtain the response measurements. Analysis of variance (ANOVA) and main effect plot are used to determine the significant parameters and set the optimal level for each parameter. The as-received and milled powders were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) and a laser particle size analyzer, respectively. The results indicate that the process control agent significantly affects (84% contribution) the mean particle size (d₅₀) while other parameters have a lower effect (16% contribution). The developed model can be used in the mechanical milling processes in order to determine the optimum milling parameters for minimum particle size.     

Effect of lubrication and green-compact shape on mechanical properties of mechanically alloyed Zn-22wt%Al powders during hot extrusion of spur gears

We investigated the extrusion behavior of mechanically alloyed Zn-22wt%Al powders with different lubricants and green-compact shapes. The mechanical alloying of powder particles was performed by planetary ball milling for 4 h, 8 h, 16 h, 32 h, and 64 h. The mechanical properties of these powders, as compacted and sintered cylindrical preforms, were estimated by uniaxial compression tests. The alloyed powder with an average particle size of 10 μm obtained after milling for 32 h had the highest compressive strength (288 MPa). Extrusions of miniature spur gears with pitch circles of 1.8 mm using the alloyed powder were carried out at different extrusion temperatures. An extrusion temperature of 310°C resulted in the highest Vickers hardness without surface defects when alloyed powder milled for 32 h was used. To investigate the effect of green-compact shape and lubricant on the dimensional accuracy and cracking regions during the first stage of hot extrusion, extrusion experiments with conical- or cylinder-type green compact shapes and BN spray or a graphite lubricant were performed at an extrusion temperature of 310°C. The results showed that the extrusion of spur gears by using the conical-shaped billet and graphite lubricant resulted in a low extrusion load, good surface roughness, a short cracking region during the first stage, and high dimensional accuracy.     

Microstructure and properties of hot compacted powders of aluminium alloys

Atomized 6061 aluminium alloy powders with and without the addition of 2 wt% Zr were milled for 80 h in a planetary ball mill and hot pressed in vacuum. The milled powders showed microhardness of about 170 HV, which increased after hot pressing up to 260 HV and up to 280 HV for powders without and with the Zr additions, respectively. Compression tests showed the high yield stress of 300 MPa obtained for the hot-pressed sample produced from the initial powders compared with ultimate compression strength of above 800 MPa for that of the milled sample and slightly higher for that with Zr additions. The effect of hot pressing on the structure of powders was investigated using a conventional analytical and high-resolution electron microscopy and high angle annular dark-field scanning transmission electron microscopy combined with energy dispersive X-ray microanalysis. The samples of initial powders hot pressed in vacuum showed a cell structure with particles of the Mg₂Si and AlFeSi phases in intercell areas. In the milled and hot-pressed sample, the homogeneous structure of small grains of size below 200 nm was observed. The AlFeSi and Mg₂Si particles with size 20–100 nm were uniformly distributed as well as the Zr rich particles in the Zr containing alloy. The Zr-rich particles containing up to 80 at% Zr were identified as a metastable fcc cubic phase with lattice parameter a = 0.48 nm.     

高能球磨-粉末冶金法制备硫化亚铁/铁基轴承材料的摩擦学性能

以Fe、C和FeS为原料,采用高能球磨工艺和粉末冶金法制备了FeS/铁基轴承材料,研究了材料的微观结构,并考察了其摩擦磨损性能。结果表明：高能球磨工艺改善了FeS颗粒的分布均匀性及其与基体的界面结合,材料力学性能高于未球磨材料;FeS属固体润滑剂且具有良好的储油特性,油润滑条件下FeS向摩擦表面转移易形成液-固润滑膜,起到了良好的减摩抗黏着作用,FeS质量分数为8%的球磨铁基轴承材料具有较好的减摩耐磨特性和较高的承载能力。     

机械合金化法制备Finemet非晶粉体的研究

利用高能卧式搅拌球磨机,研究了利用机械合金化法制备Finemet非晶粉体的工艺,研究结果表明,通过高速球磨可以得到部分非晶粉体。非晶化机制是局域熔体的快速冷却,粉体结块和粘壁,是机械合金化法制备高纯度Finemet非晶粉体的主要阻碍因素。     

机械合金化改性硫化亚铁/铜合金粉末的特性

为了解决FeS/Cu粉末冶金复合材料中FeS易团聚以及界面结合差的问题,采用机械合金化技术制备了FeS/Cu复合材料粉末。利用扫描电镜、X射线衍射仪、金相显微镜等对不同球磨时间的质量分数为6%的FeS/Cu合金粉末的混合特性、压制特性及烧结后的力学性能进行检测和分析,结果表明：机械合金化可有效改善FeS颗粒与基体合金粉末的混合均匀性,烧结后材料的密度、硬度均得到提高,FeS和Cu界面结合良好;由于FeS颗粒均匀弥散地分布在铜合金基体中,割裂了基体材料的连续性,反而使复合材料的韧性和压溃强度有所降低。     

高能球磨制备纳米级Al_2O_3/Al复合粉体过程中铝相晶粒尺寸和结构的变化

利用X射线衍射仪分析了在高能球磨制备纳米Al_2O_3/Al混合粉体过程中,球磨时间和纳米Al_2O_3含量对铝相晶粒尺寸和晶格应变的影响。结果表明:在初期短时间的球磨中,微米铝粉的晶粒尺寸迅速细化到纳米级,但随着球磨时间的进一步延长,高能球磨为晶粒融合和再生长提供了能量,使铝晶粒沿着某些晶向有长大的趋势;当Al_2O_3体积分数较低(5%)时可促进铝粉的破碎,但高含量的Al_O_3则对铝粉的球磨破碎不利。     

高能球磨制备铜/碳复合粉末及其静压固化

将粗铜粉和石墨粉按不同配比混合后进行机械合金化，球磨后粉末在1．5GPa下静压固化。采用扫描电镜对粉末及固化试样进行了显微组织观察，应用XRD对球磨后粉末进行相分析，测定了固化试样的密度和显微硬度。结果表明：粉末颗粒随含碳量的增加、球磨时间的延长而逐渐细化；固化试样的硬度与含碳量和球磨时间有关，硬度随含碳量的增加而降低；而当粉末球磨24h时，固化试样的硬度最高。     

Cryo-FIB-nanotomography for quantitative analysis of particle structures in cement suspensions

Cryo‐FIB‐nanotomography is a novel high‐resolution 3D‐microscopy technique, which opens new possibilities for the quantitative microstructural analysis of complex suspensions. In this paper, we describe the microstructural changes associated with dissolution and precipitation processes occurring in a fresh cement paste, which has high alumina and sulphate contents. During the first 6 min, precipitation of ettringite leads to a general decrease of the particle size distribution. In the unhydrated cement paste almost no particles smaller than 500 nm are present, whereas after 6 min this size class already represents 9 vol%. The precipitation of ettringite also leads to a significant increase of the particle number density from 0.294*10⁹/mm³ at t_0min to 20.55*10⁹/mm³ at t_6min. Correspondingly the surface area increases from 0.75 m²/g at t_0min to 2.13 m²/g at t_6min. The small ettringite particles tend to form agglomerates, which strongly influence the rheological properties. The particular strength of cryo‐FIB‐nt is the potential to quantify particle structures in suspension and thereby also to describe higher‐order topological features such as the particle–particle interfaces, which is important for the study of agglomeration processes.     

Generation of model diesel particles by spark discharge and hydrocarbon condensation

This study was conducted in order to generate model particles which were similar to particles in diesel emission. Spark discharge was used for carbon agglomerates and hydrocarbon condensation for particles that consist of carbon agglomerates and hydrocarbon. The size of the carbon agglomerates, whose mean size were 30 and 70 nm, ranged between 15 and 200 nm, and the total number concentration of the particles ranged from 3 to 5 × 10⁷#/cm³ as the controllable variables in spark discharge generator changed. The result of the hydrocarbon condensation experiment showed that the final sizes of the particles enlarged by condensation did not depend on the initial sizes, but the maximum condensational growth of carbon agglomerates by dodecane (C₁₂ H₂₆) condensation was 112 times the initial size of 40 nm, while the size of the agglomerates by benzene (C₆H₆) was 3.25 times its initial size.     

Effect of anneal on magnetic properties and structural state of iron powders ground in carbon-rich medium

Intense milling of iron powders in a carbon-rich liquid leads to carbonization of powder particles to concentrations of up to several weight percents, alongside the notable reduction in the dimensions of mosaic blocks and formation of a nanocrystalline structure, which results in a lower coercive force of the powder. X-ray and Mössbauer data indicate that Fe?C disordered solid solutions are formed in the regions of mosaic-block boundaries in the process of the powder milling. The anneal forms the Fe₃C ordered carbide phase from the disordered solid solution, which raises the coercive force in the powders beyond 100 A/cm.     

Role of MoS2 morphology on wear and friction under spectrum loading conditions

One of the ways by which grease is evaluated is by using a four‐ball wear test using ASTM D2266. However, actual applications may require bearings to be subjected to spectrum loading conditions. This study focuses on using ball milling to mitigate the wear from sharp edges in the MoS₂ particles. Two different blends of greases were formulated using MoS₂ in the as‐received state (unmilled) and milled MoS₂; they were tested under spectrum loading conditions where the load and frequency of the tests were treated as variables. It was found that ball milling of the MoS₂ significantly reduces the wear under spectrum loading condition both for ramp‐up and ramp‐down conditions. It was also shown that shortening the time step for both the ramp‐up and ramp‐down cycles resulted in larger wear for unmilled MoS₂ particles in comparison with milled MoS₂ particles in grease. The milling process did not play a significant role when frequency of the test was either ramped up or down. Copyright © 2015 John Wiley & Sons, Ltd.     

Magnetic Properties of Mechanically Alloyed and Annealed Powders Fe100 – X C X (X = 5 and 15 at.%)

The effect of the structural state and the phase composition on the magnetic hysteresis properties of Fe(95)C(5) and Fe(85)C(15) powders after mechanical alloying and annealing is investigated. It is shown that in the initial stage of grinding in a ball planetary mill the coercive force of the Fe–C powders is determined by the degree of defectiveness of the -Fe phase and the relative volume and dimensions of nonmagnetic graphitic inclusions in iron powder particles. As the grinding time increases, the -Fe phase goes over into a nanostructure state and carbon from graphite inclusions goes over into an amorphous Am(Fe–C) phase. After annealing on the temperature interval 300–600°C, the amorphous Am(Fe–C) phase is transformed into Fe₃C ferric carbide. The coercive force of the Fe₃C phase strongly depends on the degree of distortion of its crystal lattice and amounts to 80 A/cm for the phase with distorted lattice and 240 A/cm for the phase with equilibrium undistorted lattice. The magnetic characteristics of the powder after mechanical alloying and subsequent annealing are determined by the type, amount, and structural state of the phases containing in the samples.     

Microstructure of ball milled and compacted Co–Ni–Al alloys from the β range

Two powder alloys from the β phase region of compositions Co_28.5Ni_36.5Al₃₅ and Co₃₅Ni₃₀Al₃₅ were ball milled for 80 h in a high energy ball mill. The formation of amorphous structure was observed after 40 h of milling and further milling did not change their structure. The analytical and high-resolution transmission electron microscopy (TEM, HREM) examination of powder structure showed that nanoparticles of  L1₀ phase of size of about 5 nm were present within the amorphous matrix. The vacuum hot pressing of the milled powders under pressure of 400 MPa at 700°C for 12 min resulted in the formation of compacts with density of about 70% of the theoretical one. The additional heat treatment at 1300°C for 6 h followed by water quenching, led to significant improvement of density and induced the martensitic transformation manifested by a broad heat effect. The characteristic temperatures of the transformation were determined using DSC measurements, which revealed only small differences within the examined alloys compositions. TEM structure studies of heat-treated alloys allowed to identify the structure of an ordered β (B2) phase and L1₀ martrensite.     

Application of neural network technique to high energy milling process for synthesizing ZnO nanopowders

An artificial-neural-network (ANN) model was developed to estimate the crystalline size of ZnO nanopowder as a function on the milling parameters such as milling times and balls to powder ratio. This nanopowder was synthesized by high energy mechanical milling and the required data for training were collected from the experimental results. The synthesized ZnO nanoparticles are characterized by X-ray diffraction (XRD) and scanning electron microcopy (SEM). It was found that artificial neural network was very effective providing a perfect agreement between the outcomes of ANN modeling and experimental results with an error by far better than multiple linear regressions. An optimization model and this experimental validation of the ball milling process for producing the nanopowder ZnO are carried out.