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。     

机械合金化制备FeSiAl合金粉末的研究

采用机械合金化的方法制备了FeSiAl合金粉末样品。以硅钢粉和铝粉为原料,按摩尔分数Fe3Si0.4Al0.6配比,研究其机械合金化过程,并对机械合金化的机制进行探讨。用激光粒度仪、X射线衍射(XRD)和扫描电子显微镜分析材料的粒度、形貌和结构。研究表明,Fe3Si0.4Al0.6混合粉末球磨30h后,粉末粒径可达18μm;Fe3Si0.4Al0.6混合粉末经高能球磨20h后,形成具有bcc结构的α固溶体;球磨继续进行,合金化的粉末和晶粒不断细化。     

Thermodynamic Aspects of Nanostructured CoAl Intermetallic Compound during Mechanical Alloying

The nanostructured CoAl intermetallic compound was produced by mechanical alloying (MA) of the Co50Al50 elemental powder mixture in a planetary high energy ball mill. The ordered B2-CoAl structure with the grain size of about 6 nm was formed via a gradual reaction after 10 h of MA. A thermodynamic analysis of the process was also done. The results showed that the intermetallic compound of CoAl had the minimum Gibbs free energy compared to solid solution and amorphous states indicating the initial MA product was the most stable phase in the Co-Al system which was changed to a partially disordered structure with a steady long-range order of 0.82 at further milling. This amount of disordering caused the enthalpy of final product to show an increase of about 5.1 kJ·mol-1. Calculation of enthalpy related to the triple defect formation revealed that the enthalpy required for Al anti-sites formation was about 3 times greater than that for Co anti-sites formation.     

放电等离子烧结Ti-Al系金属间化合物

用机械合金化法(MA)制备了Ti-45% Al纳米晶合金粉末,并对其进行放电等离子烧结(SPS),烧结时间仅为5min.用D-maxIIA型X射线衍射仪、JEM-2000EX型透射电子显微镜对粉末和烧结块体的微观组织及机械性能进行了研究.研究表明:Ti和Al的粉末随着球磨时间的延长,粉末有明显的细化趋势,球磨5h即有非晶产生,球磨20h后得到接近完全非晶相;采用SPS烧结技术,在1200℃下能够制备出较高硬度的TiAl金属间化合物块体材料.     

Thermodynamic aspects of nanostructured Ti5Si3 formation during mechanical alloying and its characterization

Mechanical alloying (MA) was used to produce Ti₅Si₃ intermetallic compound with nanocrystalline structure from elemental powders. The structural changes and characterization of powder particles during milling were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), particle size analyser (PSA) and microhardness measurements. MA resulted in gradual formation of disordered Ti₅Si₃ intermetallic compound with crystallite size of about 15 nm after 45 h of milling. Also a thermodynamic analysis of the process was carried out using Miedema model. The results showed that in the nominal composition of Ti₅Si₃ intermetallic phase (X _Si ?=?0·375), formation of an intermetallic compound has the lowest Gibbs free energy rather than solid solution or amorphous phases. So the MA product is the most stable phase in nominal composition of Ti₅Si₃. This intermetallic compound exhibits high microhardness value of about 1235 HV.     

高能球磨法制备Fe_3Si合金粉末

采用高能球磨法研究了原子配比Fe75Si25的混合粉末在不同的球磨条件下的机械合金化,用X射线衍射(XRD)仪、扫描电子显微镜(SEM)表征样品的物相、晶体结构、晶粒尺寸和点阵常数,分析了Fe75Si25粉末的机械合金化机理。研究表明,球磨时间、球料比和球磨机转速对机械合金化(MA)进程有重要影响。MA 55h后可达到完全合金化,Si溶入Fe中形成α-Fe(Si)饱和固溶体,晶粒尺寸减小至7～8nm。     

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.     

Effect of Fe content on the mechanical alloying and mechanical properties of Al-Fe alloys

Al-Fe alloys with Fe contents ranging from 5 to 12 wt% are produced by a double mechanical alloying process (DMA) which consists of a first step of mechanical alloying (MA1) applied to elemental Al and Fe powders, with subsequent heat treatment of MA1 powders to promote the formation of Al-Fe intermetallic phases, and a second mechanical alloying step (MA2) to refine the intermetallic phase, and consolidation of the produced powders by combination of degassing and hot extrusion. The effect of Fe content on the process, as well as on the mechanical properties of the extruded alloys, has been extensively studied. The alloys produced by this process show excellent tensile strength and stiffness at room and elevated temperatures due to the strengthening of Al by intermetallics, as well as to the stabilization of the structure by inert dispersoids.     

高能球磨制备非晶态合金研究的进展

本文评述了目前混合基元粉末机械合金化（ＭＡ）及金属间化合物或合金粉末机械研磨（ＭＧ）制备非晶态合金的研究进展，讨论了机械合金化及机械研磨形成非晶态合金的机制。     

The effect of particle size of iron powder on α to γ transformation in the nanostructured high nitrogen Fe-Cr-Mn-Mo stainless steel produced by mechanical alloying

In this study, the effect of particle size of iron powder on α to γ transformation in the nanostructured high nitrogen Fe-18Cr-10Mn-4Mo stainless steel, produced by mechanical alloying (MA) was investigated. For this purpose iron powders with two different particle sizes were used. MA was performed under nitrogen atmosphere, using a high-energy planetary ball mill. X-ray diffraction (XRD) patterns and nitrogen analysis revealed that by decreasing the iron mean particle size, a higher transformation rate is obtained due to increase in the rate of nitrogen absorption. Moreover, nitrogen solubility in both milled samples was increased noticeably by increasing the milling time. This is believed to be due to the increase of lattice defects and development of nanostructure through MA. Variations of grain size and internal lattice strain versus milling time, for both iron particle sizes, showed that the critical ferrite grain size for austenite nucleation is less than 10 nm.     

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.     

机械合金化制备SbSn金属间化合物的研究

用机械合金化法制备SbSn金属间化合物.使用X射线衍射仪、扫描电子显微镜、透射电镜和DSC差热分析方法对Sb、Sn混合粉末经不同工艺条件合成的产物进行了分析.结果表明:机械合金化法可合成Sb-Sn金属间化合物;随着机械合金化持续进行,合金化的粉末和晶粒不断细化,晶粒内部产生很大的晶格畸变,并且球磨产生的密度和缺陷使原子扩散加快.     

Mechanical alloying and milling

Mechanical alloying (MA) is a solid-state powder processng technique involving repeated welding, fracturing, and rewelding of powder particles in a high-energy ball mill. Originally developed to produce oxide-dispersion strengthened (ODS) nickel- and iron-base superalloys for applications in the aerospace industry, MA has now been shown to be capable of synthesizing a variety of equilibrium and non-equilibrium alloy phases starting from blended elemental or prealloyed powders. The non-equilibrium phases synthesized include supersaturated solid solutions, metastable crystalline and quasicrystalline phases, nanostructures, and amorphous alloys. Recent advances in these areas and also on disordering of ordered intermetallics and mechanochemical synthesis of materials have been critically reviewed after discussing the process and process variables involved in MA. The often vexing problem of powder contamination has been analyzed and methods have been suggested to avoid/minimize it. The present understanding of the modeling of the MA process has also been discussed. The present and potential applications of MA are described. Wherever possible, comparisons have been made on the product phases obtained by MA with those of rapid solidification processing, another non-equilibrium processing technique.     

Phase transformations of NbCr2 intermetallics produced by mechanical alloying followed by hot-pressing consolidation

Mechanical alloying followed by hot-pressing consolidation has been used to produce NbCr₂ intermetallics under different conditions. High-purity Nb and Cr crystalline powders, in the relative (molar) ratio of 13:1, were milled for periods up to 100 h. This powder was vacuum-sintered at temperatures ranging from 1423 to 1573 K for 0.5 h under a pressure of 45 MPa. The phase transformations of the NbCr₂ were investigated by X-ray diffraction and scanning electron microscopy; several different phase transformations were observed. Increasing the milling time up to 100 h transforms into a mixture of C14, Nb, Cr and C15. The experimental results show that new evidence based on X-ray diffraction measurements further establishes the existence of a high-temperature C14 Laves polytype; an intermediate C36 structure for NbCr₂, reported in the literature, was not detected in this study. The relationship between the various phase transformations, based on the atomic radii and different preparation techniques, is discussed.     

Reproducibility of the Synthesis and Processing of Nanostructured Material Properties

The reproducibility or variance in the properties of nanostructured milled iron and iron alloy powders and nanostructured compacts was determined and characterized. To date, all too often the characterization of nanostructured materials has been limited to examination of one or two samples, from which it is impossible to determine the reproducibility of the reported values. In this study, multiple attritor millings were made and the variability of the macroscopic and nanostructure characteristics was determined (e.g., particle size, grain size, etc.). From a single milled powder composition, multiple hot-press compacts were made. Statistical analyses were made of the reproducibility of resulting consolidated macroscopic and nanostructured properties, such as density, hardness, grain size, and tensile/compression strength. Mechanical processing of iron powder and mechanical alloying of iron powder with aluminum, carbon, and nitrogen showed that attrition milling reliably reproduced 0.5-kg lots of nanostructured powder. Hot-pressing the milled powder also produced reproducibility nanostructured compacts. There was little or no correlation found between the milled powder properties and the compacted powder properties. Several correlations that are generally valid for large grain materials were found not to hold for nanograin compacts (e.g., between density and hardness).     

Dry sliding tribological behavior and mechanical properties of Al2024–5 wt.%B4C nanocomposite produced by mechanical milling and hot extrusion

In this paper, tribological behavior and mechanical properties of nanostructured Al2024 alloy produced by mechanical milling and hot extrusion were investigated before and after adding B₄C particles. Mechanical milling was used to synthesize the nanostructured Al2024 in attrition mill under argon atmosphere up to 50 h. A similar process was used to produce Al2024–5 wt.%B₄C composite powder. The milled powders were formed by hot pressing and then were exposed to hot extrusion in 750 °C with extrusion ratio of 10:1. To study the microstructure of milled powders and hot extruded samples, optical microscopy, transmission electron microscopy and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray spectrometer (EDS) were used. The mechanical properties of samples were also compared together using tension, compression and hardness tests. The wear properties of samples were studied using pin-on-disk apparatus under a 20 N load. The results show that mechanical milling decreases the size of aluminum matrix grains to less than 100 nm. The results of mechanical and wear tests also indicate that mechanical milling and adding B₄C particles increase strength, hardness and wear resistance of Al2024 and decrease its ductility remarkably.     

Powder Metallurgical Fabrication and Characterization of Nanostructured Porous NiTi Shape-Memory Alloy

Production of NiTi alloy from elemental powders was conducted by mechanical alloying (MA) and sintering of the raw materials. Effects of milling time and milling speed (RPM) on crystallite size, lattice strain, and XRD peak intensities were investigated by X-ray analysis of the alloy. Powder compaction and sintering time and temperature effects on pore percentage of the as-mixed and the mechanically alloyed samples were empirically evaluated. The crystallite size of the mechanically alloyed Ni₅₀Ti₅₀ samples decreased with MA duration and with the milling speed. Depending on the crystal structure of the raw materials, the lattice strain increases with the milling duration. Metallographic studies proved the existence of martensitic B19' after sintering of both the as-mixed and the mechanically alloyed samples. Its amount was, however, greater for the former. Sintering lowered the porosity of the samples; no matter what powder (as-mixed or mechanically alloyed) was used. The porosity was greater, however, for the MA powders. This difference seemed to be due to the sharper liquid phase sintering effect of the as-mixed samples.     

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.     

Synthesis of Aluminium-Cementite Metal Matrix Composite by Mechanical Alloying

Cementite powder was prepared from elemental iron and graphite powder by mechanical alloying (MA) in a specially built dual-drive planetary mill. The phase evolution, particle-size distribution, and morphology of particles were studied during 40 hours grinding period. X-ray diffraction (XRD) shows formation of cementite and other iron carbides along with elemental iron after milling, whereas after annealing only cementite is present. Initially particle size increases with milling due to ductility of iron powder and then reduces with further milling.

Al-cementite composite was synthesized by mixing cementite with Al powders, and then by hot pressing or cold compaction and sintering. XRD analysis of Al-Fe₃C composite shows Fe₃C, FeAl, Al, and other iron carbides along with Al₄C₃ after sintering. Scanning electron microscope (SEM) micrograph of hot-pressed samples shows excellent compatibilility between Al matrix and cementite particles.     

Amorphization and nanocrystalline Nb3Al intermetallic formation during mechanical alloying and subsequent annealing

In this paper the formation as well as the stability of Nb₃Al intermetallic compounds from pure Nb and Al metallic powders through mechanical alloying (MA) and subsequent annealing were studied. According to this method, the mixture of powders with the proportion of Nb-25 at% Al were milled under an argon gas atmosphere in a high-energy planetary ball mill, at 7, 14, 27 and 41 h, to fabricate disordered nanocrystalline Nb₃Al. The solid solution phase transitions of MA powders before and after annealing were characterized using X-ray diffractometry (XRD). The microstructural analysis was performed using scanning electron microscopy (SEM) as well as transmission electron microscopy (TEM). The results show that in the early stages of milling, Nb(Al) solid solution was formed with a nanocrystalline structure that is transformed into the amorphous structure by further milling times. Amorphization would appear if the milling time was as long as 27 h. Partially ordered Nb₃Al intermetallic could be synthesized by annealing treatment at 850 °C for 7 h at lower milling times. The size of the crystallites after subsequent annealing was kept around 45 nm.