机械合金化过程中Fe-Al合金粉末的组织演变

将纯Fe粉和Al粉按原子比Fe∶Al=60∶40混合后,在行星式高能球磨机中进行机械合金化,采用X射线衍射仪、扫描电镜、透射电镜和硬度仪研究球磨过程中Fe-Al合金粉末相结构、晶粒尺寸、表面形貌、截面形貌和硬度的演变规律。结果发现,球磨24 h后,Al原子全部固溶于Fe晶格中,形成Fe(Al)过饱和固溶体,随着球磨时间的增加,晶粒尺寸呈现先快后慢的减小趋势,球磨36 h后合金粉末的晶粒尺寸小于100 nm。粉末内部组织为层状结构,且随着球磨时间延长层片厚度不断减小,球磨36 h后层状结构全部消失,获得组织均匀的纳米晶Fe-Al合金粉末。随着球磨时间延长,Fe-Al合金粉末的硬度不断增加,球磨36 h后合金粉末的硬度约为405 HV0. 025。球磨Fe(Al)固溶体合金粉末在500℃热处理转变为有序Fe Al金属间化合物。     

机械合金化制备纳米晶C/Cu复合粉末的研究

将粗铜粉和石墨粉按不同配比混合后进行机械合金化,并对机械合金化粉末的物相、合金化特征、晶粒尺寸进行了分析研究。结果表明,在球磨过程中,随球磨时间延长有越来越多的C原子溶入Cu的晶格,点阵常数随球磨时间和粉末中石墨含量的增加而增加,球磨24h时达到最大值,继续球磨,点阵常数略有降低。机械合金化可以使晶粒细化并产生大量孪晶位错和纳米晶界面,有利于原子扩散形成过饱和固溶体和非晶,C/Cu复合粉末球磨30h后晶粒尺寸可达到22nm。     

MA法制备Fe83Nb7B9Cu1纳米晶粉末及其热稳定性

利用高能球磨法在Fe Nb B Cu体系中获得纳米晶粉末 ,研究了机械球磨过程中产物的组织结构、α Fe相平均晶粒尺寸及其热稳定性。结果表明 :采用Fe 2 0B中间合金粉末代替B粉并未明显影响机械合金化动力学过程 ;球磨至 5h时 ,即可获得平均晶粒尺寸约 18nm的α Fe单相过饱和固溶体 ,其后延长球磨时间 ,晶粒尺寸缓慢减小 ,至 45h后 ,平均晶粒尺寸减小到 9nm。退火处理后的XRD分析表明 ,α Fe过饱和固溶体从 10 0℃开始发生结构弛豫现象 ,738.8℃后则发生了相转变 :α Fe过饱和固溶体→α Fe固溶体 Fe3 B FeB ,在 5 5 0℃以内退火 ,纳米晶粒长大不明显 ,在 770～ 95 0℃范围内退火 ,晶粒开始明显长大 ,但晶粒尺寸仍处于纳米级范围。     

机械合金化制备Ta-10%Al纳米晶过饱和固溶体

利用机械合金化的方式制备了组成为Ta-10%Al(质量比)的纳米晶过饱和固溶体。以XRD和SEM为表征手段,研究了球磨时间对Ta-10%Al纳米晶过饱和固溶体产生的影响,并对Ta-10%Al纳米晶过饱和固溶体形成的热力学机理进行了研究。结果表明,随球磨时间增加,Al逐渐溶入Ta中。当球磨时间达到48 h后,Al完全固溶进Ta中形成Ta-10%Al纳米晶过饱和固溶体,晶粒尺寸和微观应力分别为84.3 nm和0.285%。延长球磨时间导致Ta-10%Al纳米晶过饱和固溶体晶粒细化且微观应力增加,过长的球磨时间可能引发合金粉末的团聚。以Miedema半经验模型为依据,建立了机械合金化过程中的热力学模型,计算结果显示,以机械合金化为手段制备Ta-10%Al纳米晶过饱和固溶体的主要驱动力来源于热力学驱动。     

高能球磨制备纳米级WC/Cu复合粉末的研究

利用XRD、SEM等分析研究了高能球磨时间对WC／Cu复合粉末结构、形貌及相的影响。结果表明，随球磨时间的延长复合粉末发生细化达到纳米级粒度，球磨24h可获得稳定晶粒尺寸，最小晶粒尺寸为21．5nm。其中WC粉末晶粒细化速率较Cu的慢；球磨过程中，有少量的WC固溶于Cu中，形成Cu(WC)固溶体。     

机械合金化制备W-Ni-Fe纳米-非晶材料

按照80．7W-13．2Ni-6．1Fe的原子分数．采用机械合金化(MA)方法，制备了W-Ni-Fe合金纳米晶和非晶相的混晶结构。结合XRD，利用近似内标法计算了球磨不同时间球磨粉中残留晶体W的体积分数和非晶相中的W含量，并分析了球磨过程中非晶形成的机制。结果表明：随球磨时间的延长，W晶粒不断细化．球磨60h，钨晶粒尺寸可达到10nm-20nm，非晶相的形成过程主要是Ni(Fe)首先溶入W中形成过饱和固溶体，球磨20h后形成W-Ni(Fe)非晶。过饱和固溶体的形成是由于携带较大晶界存储能的小粒子不断溶入W中，计算得到可固溶的临界Ni粒子尺寸约为3nm。由于Fe污染不断溶入W中，在球磨过程中，残留晶体W的体积分数不断减少．而非晶相中的W-Ni(Fe)比例基本保持恒定，为63W-37Ni(Fe)。     

机械化学还原法快速制备Mo5Si3-Al2O3纳米复合粉体（英文）

以MoO3粉、Mo粉、Si粉及Al粉为原料,采用机械合金化法合成了纳米Mo5Si3-20%Al2O3(质量分数)复合粉体。采用XRD、SEM、TEM和DTA等对复合粉体在球磨过程中结构变化进行了研究。结果表明:球磨10h后合成的Mo5Si3-20%Al2O3复合粉体,反应以爆炸模式进行。球磨30h后,Mo5Si3和Al2O3的晶粒尺寸分别为36.3nm和21.9nm。随着球磨时间的延长,Mo5Si3和Al2O3的晶粒尺寸变小,衍射峰宽化程度降低。DTA和XRD分析结果表明,复合粉体具有好的热稳定性,球磨30h后再在1000℃退火1h后复合粉体没有发生物相转变。     

MAGNETIC PROPERLIES AND STRUCTURE OF A MIXTURE OF α-Fe and Fe_3N DURING MECHANICAL ALLOYING PROCESS

利用X射线衍射研究了α-Fe与Fe3混合粉末机械合金化过程中结构的变化．并测量了球磨不同时间后其饱和磁化强度的变化结果表明,随着球磨时间的延长,Fe3N相迅速分解直至消失,N原子部分固溶于α-Fe中,24h后可形成稳定的α-Fe（N）过饱和固溶体,其中N的质量分数约为0．290％-0．346％．随着球磨时间的延长,α-Fe的晶粒尺寸逐渐减小,24h后趋于定值,约为8nm．球磨引起样品中Fe原子周围N原子位置的变化,使得球磨过程中混合粉末的饱和磁化强度开始时降低,5h后又有所增加,24h后达到一定值     

高能球磨制备Al-Pb-Si-Sn-Cu纳米晶粉末的特性

通过机械合金化制备了Al-15％Pb-4％Si-1％Sn-1．5％Cu(质量分数)纳米晶粉末。采用X射线衍射(XRD)，扫描电镜(SEM)和透射电镜(TEM)对不同球磨时间的混合粉末的组织结构、晶粒大小、微观形貌以及颗粒中化学成分分布情况进行了研究。结果表明混合粉末经过球磨后形成了纳米晶，其组织非常均匀。球磨对Pb的作用效果明显大于对Al的作用效果，经过40h球磨后Pb粒子达到40nm，而Al在球磨60h后晶粒为65nm；经球磨后，Cu和Si固溶于Al的晶格中，而Sn则固溶于Pb晶格中，并且Al和Pb发生了互溶，形成了Pb(Al）超饱和固溶体；在球磨过程中硬度高的脆性粒子Si难于完全实现合金化。     

3Cu-2Mg-Al混合粉末球磨过程的机械力化学效应

通过X射线衍射仪,电子显微镜和Pulverisette5行星式球磨机研究了3Cu-2Mg-Al粉末在球磨过程中的机械化学变化.结果表明,随球磨时间的延长,3Cu-2Mg-Al粉末晶粒尺寸减小,显微应变和有效温度系数增加;晶粒尺寸与有效温度系数和显微应变呈逆变关系,显微应变随有效温度系数增加而增大;球磨30 h后,Mg衍射峰完全消失,球磨至60 h,Al衍射峰也完全消失,Cu衍射峰进一步宽化,此时,Cu衍射峰位置向小角度偏移,形成了Mg和Al在Cu中的过饱和固溶体;球磨90 h后,有新相Mg32Al47Cu7生成.     

Mechanical alloying of Mo—Si—Fe powders

Mechanical milling behavior of Mo-Si-Fe powders was investigated u sing XRD, SEM and TEM techniques. The mixtures of elemental molybdenum (>99%), s ilicon (>99%) and iron (>98%) powders with a stoichiometry of Mo5-xFe xSi3 (x=0.5, 1, 2) were milled in a planetary mill for up to 195 h. For all three powder mixt ures, high-energy milling of 60h led to formation of the Mo(Fe, Si) supers aturated solid solution (Moss); and to a remarkable expansion of the solub ility of Fe, Si in molybdenum. The transformation of Moss to an amorphous phase was identified after longer time milling. In the milling process, the grain size of Mo (Fe, Si) decreased gradually and the internal stress increased linearly. After 40 h milling, the grain size was reduced to about 11 nm. SEM analysis of milled powders showed that the particle size increased initially with milling time. After 195 h milling, particles exhibited a spherical morphology and the particle size were reduced to about 100 nm.     

Ultramicro molybdenum nitride powder prepared using high-energy mechanochemical method

Using the specially designed mechanochemical ball-mill equipment, ultramicro molybdenum nitride powders were prepared from pure molybdenum powders in ammonia atmosphere at room temperature by high-energy ball milling. The structure and the particle size of the powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The results show that the mass ratio of grinding media to powder was 8:1, after milling for 30h the Mo2N of fcc structure was obtained, and the average particle size of the powders was around 100 nm. It is found that the chemisorption of ammonia onto the fresh molybdenum surfaces created by milling was the predominant process during solid-gas reaction, and the energy input due to introduction of highly dense grain boundaries and lattice defects offered the activation energy for the transition from Mo-N chemisorption to molybdenum nitride. In addition, the change of Mo electronic undersaturation induced by the grain refining accelerated the bonding between Mo and N. The mechanism model of whole nitriding reaction was given. During the high-energy ball milling processing, the rotational speed of milling played a critical role in determining the overall reaction speed.     

Mechanical alloying behaviors of Mo-Si-B-based alloy from elemental powders under different milling conditions

Elemental powder mixtures with the composition of Mo-12Si-10B-3Zr-0.3Y(at%)were milled in a planetary ball mill using hardened stainless-steel milling media under argon atmosphere.Effects of milling time,milling speed,process control agent,ball-to-powder ratio and milling ball size on the mechanical alloying processes were investigated from the points of morphology,internal structure,grain size,microstrain,phase constituent and issolution of solute atoms.It is shown that under all conditions,the microstructural evolutions of mechanically milled powder particles are similar.The morphological evolution can roughly be divided into five stages:individual particle,irregular blocky composite particle,flakeshaped particle,agglomerate and single particle.The internal structure generally undergoes five stages:individual particle,coarse lamellar structure,fine lamellar structure,non-uniformly mixed structure and plum-pudding structure.Regardless of exceptional cases,the grain size of Moss decreases and its microstrain increases with the increase in milling time.Si and Zr atoms are dissolved into Mo gradually with the progress of milling.However,the evolutionary rates change significantly with milling conditions.The most significant influencing factor among different milling conditions is the input power from the mill to the powders,which plays a decisive role in the milling process.     

Microstructural evolution of mechanically alloyed Mo–Si–B–Zr–Y powders

Elemental powder mixtures with compositions of Mo–13.8Si, Mo–20B and Mo–12Si–10B–3Zr–0.3Y (at.%) were respectively milled in a high energy planetary ball mill at a speed of 500 rpm. Microstructural evolution of powder particles during milling processes was evaluated. The results show that B can hardly be dissolved into Mo under present milling conditions and the additions of B and Si both accelerate the refining rate of Mo crystallites. For Mo–12Si–10B–3Zr–0.3Y system, the morphology and internal structure of powder particles change significantly with milling time. After 40 h of milling, an almost strain-free super-saturated molybdenum solid solution with a grain size of about 6.5 nm forms. The grain refinement mechanism and dissolution kinetics of solute atoms are highlighted. Both thermodynamic calculation and experimental results reveal that for the present alloy composition it is more favorable to form solid solution than amorphous phase.     

Structural and magnetic properties of nanostructured Fe50(Co50)-6.5 wt% Si powder prepared by high energy ball milling

This work investigates the effects of 6.5 wt% Si addition and milling times on the structural and magnetic properties of Fe₅₀Co₅₀ powders. For this purpose, at first the elemental Fe and Co powders were milled for 10 h to produce Fe₅₀Co₅₀ alloy and then Si was added and the new product was milled again for different times. The microstructural and magnetic properties were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). The results show that the minimum crystallite size of the as-milled powders (∼12 nm) has been achieved after introducing Si and milled for 8 h (total milling time of 18 h). Also an amount of 188 emu/g has been achieved for M_s. This amount of M_s is higher than most of those which have been already reported for M_s of different Fe-Si systems.     

Softening behaviour of nanostructured Al–14 wt% Zn alloy during mechanical alloying

Al and Zn elemental powder mixtures were subjected to high-energy milling to produce Al–14 wt% Zn alloy. The milled powders were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and microhardness measurement. The Al and Zn grain sizes were estimated from broadening of XRD peaks using Williamson–Hall formula. The results showed that in early stage of milling the solubility of Zn in Al is extended compared to the equilibrium value which is accompanied by a decrease in lattice parameter of the Al matrix. However, after longer milling times, decomposition of Al(Zn) supersaturated solid solution appeared to occur leading to an increase in Al lattice parameter and also a decrease in hardness value of as-milled powder. The final product of milling includes both Al and Zn phases having a grain size of 40 nm and 20 nm, respectively.     

AMORPHIZATION TRANSFORMATION BY MECHANICAL ALLOYING IN THE Mo-Si SYSTEM

1.IntroductionInrecelltyears,MoSiZhasattractedconsiderableattentionasapotentialhigh-temperaturestructuralmaterial.Thecombinationofhighmeltingpoint(2030"C),moderatedensity(6.24gcm--'),excellentoxidationresistance,andhighmodulusatelevatedtemperaturemakesMoSiZoneofthemostpromisingmatrixphasetobeusedattemperaturesupto1600oC[l].Anothermolybdenumsilicide,Mo5Si3,hasbeenproposedasapotentialreinforcementforMoSt,[1,2].AmongawidevarietyofprocessingtechniquesutilizedtosynthesizeMoSt2,mechanicalalloy…     

Nanophase intermetallic FeAl obtained by sintering after mechanical alloying

The preparation of bulk nanophase materials from nanocrystalline powders has been carried out by the application of sintering at high pressure. Fe–50 at.%Al system has been prepared by mechanical alloying for different milling periods from 1 to 50 h, using vials and balls of stainless steel and a ball-to-powder weight ratio (BPR) of 8:1 in a SPEX 8000 mill. Sintering of the 5 and 50 h milled powders was performed under high uniaxial pressure at 700 °C. The characterization of powders from each interval of milling was performed by X-ray diffraction, Mössbauer spectroscopy, scanning and transmission electron microscopy. After 5 h of milling formation of a nanocrystalline α-Fe(Al) solid solution that remains stable up to 50 h occurs. The grain size decreases to 7 nm after 50 h of milling. The sintering of the milled powders resulted in a nanophase-ordered FeAl alloys with a grain size of 16 nm. Grain growth during sintering was very small due to the effect of the high pressure applied.     

超细WC-Co硬质合金的制备与性能研究

利用高能球磨法制备纳米级WC-Co混合粉末,采用脉冲电流烧结技术进行烧结。用能谱分析仪(EDX)对球磨后的粉末进行成分分析,用X射线衍射(XRD)对比分析球磨前后WC-Co混合粉末的衍射峰变化,用透射电子显微镜(TEM)和扫描电子显微镜(SEM)对所制备的粉末及烧结材料进行了组织形貌观察,并测定了烧结试样的硬度。结果表明:随着球磨时间的延长,WC-Co纳米粉末的粒度逐渐变小,当球磨时间超过30h后获得了粒度为100nm以下的WC-Co纳米粉末。脉冲电流烧结后获得超细WC-Co硬质合金,与传统的WC-Co硬质合金相比,超细WC-Co硬质合金具有更高的硬度(HRA92.5～94)和耐磨性。另外通过实验获得了最佳的烧结工艺参数。