基于外场辅助的机械合金化研究

机械合金化（MA）技术作为一种制备纳米材料的有效方法已获得广泛的应用。把机械合金化过程中的磨球机械能与其它物理能有机地结合起来,能够增强对粉末的作用,有效提高机械合金化效率。本文简单回顾了机械合金化的发展,对外加物理场辅助作用下的几种高能球磨工艺进行了详细分析。采用物理能辅助机械球磨,从而使粉末得到复合作用或活性激活,是机械合金化效率提高的原因。     

高能球磨制备氮化铝粉体的研究进展

综述了应用高能球磨技术制备氮化铝粉体的研究进展。高能球磨机械力活化效应可以降低后续合成氮化铝的碳热还原反应温度,其主要机制是球磨导致氧化铝粉体的细化以及晶格畸变的积累,进而降低了反应的热力学能垒。而球磨使得原料粉体均匀混合,增加动力学扩散通道并不是低温合成氮化铝的主要原因。利用等离子体辅助高能球磨技术可以高效活化氧化铝粉体,显著降低后续反应的激活能,这有望成为制备氮化铝粉体的一条新途径。     

高能球磨Mg/B复合粉末的特性

对化学计量比的Mg/B原始粉体进行高能球磨,通过扫描电镜SEM和能谱分析EDX对球磨前后的粉末进行观察,对球磨过程中复合粉末的组织形貌和成分分布的变化进行了研究.结果表明:随着球磨时间的延长,Mg粉明显细化,B粉在Mg粉中的均匀弥散分布程度很好.     

等离子体辅助球磨制备表面修饰片状纳米Cu粉及摩擦学性能

以硬脂酸为过程处理剂,采用等离子体辅助球磨制备表面修饰片状纳米Cu粉,并测试其摩擦学性能。结果表明:在等离子体的快速加热及电致塑性效应协同作用下,Cu粉呈现出超塑性而发生剧烈形变,辅助球磨5h制备的片状纳米Cu粉一次颗粒厚度在20nm左右。等离子体辅助球磨使片状纳米Cu粉体表面吸附并化学键合了非极性基团,Cu粉获得亲油疏水表面特性,在40CA船用润滑油中具有良好的分散性。片状纳米Cu粉严重的变形使其具有极高的活性,在摩擦过程中容易吸附铺展在摩擦副表面,使复合油有更好的抗磨性能。在高载荷、高转速工况下,片状纳米Cu粉显示出良好的减摩自修复效果,有效提高了润滑油的极压抗磨性能。     

HDDR处理的Sm2Fe16Ti1Nx化合物高能球磨的研究

在用HDDR法制备Sm2Fe16Ti1Nx氮化物过程中,研究了高能球磨对氮化物粉末的形貌、物相结构及磁性能的影响.发现高能球磨Sm2Fe16Ti1Nx氮化物使粉末颗粒细化的过程可描述为大粉末颗粒→压延成层片状→断裂成短棒状及球形颗粒→压延成层片状→断裂成球形小颗粒,并在球磨一定时间后使粉末中的Sm2(FeTi)17Nx主相完全非晶化,α-Fe含量增高且没有非晶化.球磨后粉末的矫顽力随着球磨时间的延长而降低,而剩磁在球磨短时间时降低,再延长球磨时间又增高,在球磨较长时间到Sm2(FeTi)17Nx主相完全非晶化后又使剩磁降低,最高磁场下的磁化强度值则随着球磨时间的延长而增加.手研磨后粉末的矫顽力随研磨时间的延长而逐渐升高而剩磁及最高场下磁化强度值变化不大.     

高能球磨法制备不锈钢-TiC纳米复合粉末的研究

在真空条件下采用高能球磨法以不锈钢粉末、钛粉和碳粉为原料制备了不锈钢-TiC超细复合粉末.X射线、扫描电子显微镜、比表面积评价等分析技术被用来对球磨过程中粉末的微观状态进行了分析.结果表明,随着球磨时间的增加,不锈钢复合粉末逐渐细化,用X射线衍射方法计算的最终晶粒可达到20nm.同时,钛粉和碳粉在球磨过程中发生反应形成TiC,可获得纳米级的不锈钢-TiC复合粉末.     

稀土对SiC纳米粉体机械合金化形成的影响

采用稀土作为添加剂,利用高能球磨方式将Si、c的混合粉体合成纳米尺寸的SiC,利用扫描电镜观察经球磨后的粉体形貌,用X射线衍射仪对球磨后的粉体进行物相分析.结果表明:添加一定量的稀土可促进SiC的合成并加快粉体的细化过程.     

高能球磨固态扩散反应研究

从扩散理论出发,结合结合Ａｌ－Ｃｕ合金高能球磨实验结果,分析了高能球磨过程中的扩散特点,提出了固态合成反应模型并进行了分析计算,结果表明,高能球磨过程中固态反应能否发生取决于体系在球磨过程中能量升高程度,而反应完成与否则受体系中的扩散过程控制,即受制于晶粒细化攻粉末碰撞温度。     

等离子体辅助球磨活化对Al_2O_3+C合成AlN固-固反应的影响机制

利用介质阻挡放电等离子体辅助球磨和普通球磨分别对Al_2O_3+C混合物料进行活化,研究等离子体辅助球磨活化后Al_2O_3+C合成AlN的碳热还原反应机制。结果表明,等离子体辅助球磨30h的Al_2O_3+C,在N2气氛中1 400℃下保温4h,Al_2O_3即可全部转化为AlN,Al_2O_3+C的碳热还原反应符合固-固反应机制。相对于球磨活化单一的Al_2O_3粉末,等离子体辅助球磨Al_2O_3+C混合粉末可以缩短10h的球磨活化时间,这主要是由于在等离子体与球磨的协同作用下,有利于Al_2O_3与C形成适于固-固反应的均匀互溶的精细复合结构,使得反应扩散通道增加,平均扩散路径缩短,这在动力学方面大大促进了Al_2O_3+C的碳热还原反应,并促使反应按照固-固机制进行。     

纳米偏硼酸钙/还原石墨烯润滑添加剂的制备及摩擦学性能

为了研究表面改性纳米偏硼酸钙/还原石墨烯润滑添加剂的合成方法,以偏硼酸钙、还原石墨烯为原料,油酸为修饰剂,利用等离子体辅助球磨制备纳米偏硼酸钙/还原石墨烯复合粉体,并测试其摩擦学性能.采用扫描电镜、透射电镜、X射线衍射仪和红外光谱仪对纳米偏硼酸钙/还原石墨烯复合粉体进行形貌观察;采用形状测量激光显微镜、扫描电镜对摩擦副表面进行测试;采用MOAⅡ油液分析光谱仪对摩擦油样进行检测.结果表明:在钢球机械研磨和等离子体热效应的耦合作用下,等离子体辅助球磨10 h的偏硼酸钙与还原石墨烯继续球磨10 h后,被细化为10 nm左右的颗粒状,并均匀地负载于还原石墨烯上.等离子体快速加热使得偏硼酸钙粉体表面发生热爆,部分偏硼酸钙飞溅在还原石墨烯上,并随即被其包裹为球状复合结构.等离子体辅助球磨10 h为偏硼酸钙表面引入羧基基团,并在后续球磨中与还原石墨烯表面的羟基发生酯化反应,原位完成油酸对偏硼酸钙和还原石墨烯的表面改性,使得纳米偏硼酸钙/还原石墨烯复合粉体在5W-40型机油中具有良好的分散性.在摩擦过程中,比表面积大的还原石墨烯不断吸附在摩擦表面,同时被还原石墨烯包裹为球状的纳米偏硼酸钙粒子,使摩擦副表面产生多活动中心的滚动摩擦,从而有效改进复合油的减摩抗磨性能.     

Structural characterization of nanostructured Fe-8P powder mixture

Nanostructured Fe-8P (wt%) powder mixture was prepared by high energy ball milling in a planetary ball mill (Fritsch P7) under argon atmosphere. The morphology of the particles, the phase identification and the alloying evolution process as a function of milling time are studied by scanning electron microscopy (SEM), X-ray diffraction (XRD) and 57Fe M?ssbauer spectrometry (MS), respectively. Refinement based on Rietveld method of the XRD patterns and the M?ssbauer spectra analysis show that the Fe(x)P (1 < x < 2) and Fe2P phosphide phases are the main product after 3 h of milling (approximately 10%). From the XRD Rietveld refinement, it is observed that the Fe2P phase disappears completely after 12 h of milling, while the Fe3P nanophase appears after 9 h and remains for larger milling duration. The lattice structure distortion is evidenced by the lattice parameter changes of the milled products. A two structure state of the alpha-Fe(P) solid solution: alpha-Fe1 and alpha-Fe2 is confirmed by both the XRD and MS measurements. After milling for 21 h, a mixture of a disordered two phase alpha-Fe(P) solid solution, Fe3P nanophase and a small amount of a paramagnetic FeP phosphide phase (approximately 2%) is obtained.     

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。     

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。     

Refining of copper powder by a novel micro-abrasive milling method conducted in the air

The pure copper powder was milled by conventional high-energy ball milling (CM) and micro-abrasive milling (MAM) methods in the air or vacuum. The refining behavior of copper powder milled using these different methods has been studied, and the morphologies, microstructures, compositions, and properties of the milled powders have been thoroughly investigated. The results show that, as compared to CM, the MAMed copper powder had a better refinement behavior and contained a smaller number of agglomerates. After milling in the air for 30 h by MAM, whole copper powder was converted into Cu₂₊₁O. In addition, under the synergistic effects of micro-abrasion and exposure to oxygen, the Cu₂₊₁O powder was soft-agglomerated and had a specific surface area of 15.1031 m²/g and an average size of 375.4 nm. During the dispersion process, Cu₂₊₁O was partly converted into CuO and the microstructural evolution characteristics were disclosed. The dispersed powder had an average particle size of 179.5 nm. The refining mechanism of the copper powder prepared by the micro-abrasive milling method was also discussed.     

Mechanical processing of Fe powders

Fe powders were mechanically processed by ball milling. The average size of coherent diffraction domains and the average strain content were determined by X-ray diffraction. A mathematical model was developed to describe the microstructural refinement process as a function of the number of collisions and to estimate the amount of powder effectively processed at individual collisions. The density of dislocations was also estimated. The obtained values suggest that Fe powders can locally undergo extremely severe deformation conditions.     

X-ray line profile analysis of the ball-milled Fe–30Co alloy

This work deals with the microstructural properties of the Fe–30Co alloy prepared by ball milling of elemental iron and cobalt powders. The obtained mixed powder has been characterized by means of scanning electron microscope, X-ray microanalysis, laser diffraction, X-ray diffraction and microhardness measurements. X-ray line profile analysis based on the Rietveld method and adopting two different models has been used for the microstructural study. The refinement of the X-ray patterns shows that after 3 h of high energy milling the Fe(Co) is formed. The obtained Fe(Co) solid solution is characterized by body centered cubic structure with a lattice parameter a = 0.28564 ± 0.00004 nm and an ellipsoidal crystallite and microstrain field. The dissolution of cobalt in iron matrix is accompanied by the compression of the crystalline lattice by 0.37%. The progress of milling process produces an increase of the Debye–Waller factor and the dislocation density leading to the hardening of the powder. The variation of microhardness with milling time shows a change in hardening mechanisms.     

Fe-Cu 系机械球磨合金化研究

目的为了实现Fe粉和Cu粉的合金化及观察其过程变化。方法采用机械球磨的方法,利用扫描电子显微镜等仪器,对球磨过程中的组织演变过程及微观形貌进行了研究。结果通过球磨得到了十几个纳米尺寸的晶粒。结论通过球磨可以得到过饱和固溶体。     

Fabrication of ultrafine W – Cu powders by mechanical alloying

Abstract

Ultrafine composite powders of W – 15 wt-%Cu, W – 25 wt-%Cu, and W – 35 wt-%Cu have been fabricated by mechanical alloying. The effects of type of mill, process control agent, temperature of milling, and ball/powder ratio on the final products have been evaluated. The results show that the planetary ball mill possesses a higher impact energy intensity than that of the vibratory ball mill. The optimum milling time is confirmed by the formation of a nanocrystalline microstructure in the planetary ball mill after optimisation of the milling parameters. A steady state between cold welding and fracture is attained with a milling time of up to 25 h in the planetary ball mill under optimised conditions. Crystallites with sizes of 7 – 8 nm for W – Cu composite powders have been obtained after 25 h of ball milling. The powders obtained after mechanical alloying have been characterised in terms of their size, shape, phase constitution, and microstructural features using X-ray diffraction and scanning electron microscopy.     

机械合金化法制备Cr掺杂Fe-Si合金

采用高能行星式球磨机制备了Cr掺杂Fe-Si混合粉,用X射线衍射（XRD）测试研究Cr掺杂Fe-Si合金的机械合金化过程,实验结果表明,随着球磨强度的增加,Fe、Cr、Si粉末通过原子扩散实现机械合金化,最佳的球磨工艺参数为：球磨时间35h、球磨机转速360r/min、球料比40：1。     

Processing of Cu-Fe and Cu-Fe-SiC nanocomposites by mechanical alloying

The Cu-Fe and Cu-Fe-SiC nanocomposite powders were synthesized by a two step mechanical alloying process. A supersaturated solid-solution of Cu-20 wt% Fe was prepared by ball milling of elemental powders up to 5 and 20 h and subsequently the SiC powder was added during additional 5 h milling. The dissolution of Fe into Cu matrix and the morphology of powder particles were analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. It was found that the iron peaks in the XRD patterns vanish at the early stages of mechanical alloying process but the dissolution of Fe needs more milling time. Moreover, the crystallite size of the matrix decreases with increasing milling time and the crystallite size reaches a plateau with continued milling. In this regard, the addition of SiC was found to be beneficial in postponing the saturation in crystallite size refinement. Moreover, the effect of SiC on the particle size was found to be significant only if it is added at the right time. It was also found that the silicon carbide and iron particles are present after consolidation and are on the order of nanometer sizes.