机械合金化过程中Fe50Al50二元系的结构演变

利用高能球磨和后续热处理技术制备纳米晶Fe50Al50(摩尔分数,%)合金粉体.采用X射线衍射、透射电镜和扫描电镜对元素混合粉在机械合金化过程中的结构演变及热处理对合金化粉体结构的影响等进行分析,讨论其机械合金化合成机制.结果表明:球磨过程中Al向Fe中扩散,形成Fe(Al)固溶体.机械合金化合成Fe(Al)遵循连续扩散混合机制;球磨30 h后,粉体主要由纳米晶Fe(Al)构成,晶粒尺寸5.65 nm;热处理导致Fe(Al)纳米晶粉体有序度提高,转变为有序的B2型FeAl金属间化合物,粉体的晶粒尺寸增大,但仍在纳米尺度范围.     

机械合金化及热处理过程中Ti50C50二元系统的结构演变

使用X射线衍射仪（XRD）、透射电子显微镜（TEM）研究了Ti50C50元素混合粉在机械合金化过程中的结构演变以及热处理对粉体结构的影响,讨论了TiC机械合金化合成机制。研究结果表明,机械合金化合成TiC遵循逐渐扩散反应机制,反应首先形成纳米晶Ti（C）粉体,球磨10h析出TiC,随着球磨过程的进行,TiC的量逐渐增多,品格常数增加,晶粒尺寸降低。球磨80h后,粉体主要由纳米晶TiC构成,晶粒尺寸6nm,但仍有少量的Ti（C）剩余。热处理促进残余的Ti（C）转变成TiC,同时导致TiC粉体晶粒生长,晶粒尺寸增大,晶格畸变程度降低,有序度提高。     

机械合金化及热处理过程中Ti33B67二元系统的结构演变

采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)及粉体粒度仪研究了Ti33B67元素混合粉在机械合金化过程中的结构演变、球磨后粉体的颗粒形态与粒度分布以及热处理对粉体结构的影响,讨论了TiB2机械合金化合成机制。实验结果表明,机械合金化合成TiB2遵循逐渐扩散反应机制,过程如下：Ti B→Ti(B）纳米晶→Ti(B)非晶→TiB2纳米晶。球磨20h析出TiB2,球磨60h后完全转变为TiB2。TiB2粉体颗粒基本呈球形,具有比较宽的粒径分布,平均粒度d0.5为0．964μm。热处理导致TiB2粉体晶粒生长,晶粒尺寸增大,品格畸变程度降低,有序度提高。     

机械合金化过程中Fe75 Al25二元系统的结构演变

采用X射线衍射仪、差式扫描量热仪等研究机械合金化过程中Fe75Al25元素混合粉的结构演变及热处理对粉体结构的影响。研究表明：球磨过程中，Al向Fe中扩散，直至Al完全溶入Fe中形成非平衡过饱和固溶体Fe(Al)。球磨过程中，Fe75Al25元素混合粉晶粒细化呈现先快后慢的趋势，球磨25h后的晶粒尺寸为6．9nm。Fe75Al25元素混合粉在球磨后的热处理过程中，由无序的Fe(A1)固溶体向有序的DO3-Fe3Al金属间化合物转变。     

原位TiB2/Fe3Al基纳米复合材料的合成及其晶粒生长动力学(Ⅱ)——热处理过程中机械合金化Fe-Al-Ti-B四元粉体的结构演变与晶粒生长动力学

研究了机械合金化合成的Fe-Al-Ti-B四元粉体在800-1100℃等温热处理过程中的结构演变及晶粒生长动力学,讨论了晶粒生长机制。研究表明,采用机械合金化加后续热处理工艺可以合成原位TiB2/Fe3Al基纳米复合材料粉体。球磨80h的Fe-Al-Ti-B四元粉体在热处理过程中Fe(Al,Ti,B)分解形成纳米晶DO3-Fe3Al及TiB2两个组成相。随热处理温度的升高,Fe3Al晶粒生长由主要受晶界扩散控制过渡到主要受晶格扩散控制。在热处理过程中,Fe3Al晶粒生长的动力学方程为:K=1.5×10-5exp(-578.7×103/RT),晶粒生长受到明显的抑制,原位TiB2/Fe3Al基纳米复合材料粉体的热稳定性高。     

机械合金化及真空热压制备纳米晶Fe3Al的组织及性能

采用机械合金化(MA)及热压烧结工艺制备纳米晶Fe3Al块体材料。采用X射线衍射、透射电镜、扫描电镜等对MA粉体及热压块体的相及显微组织进行分析,并对热压块体的力学性能及断口形貌进行了测试分析。结果表明:Fe72Al28混合粉在球磨过程中,Al逐渐溶入Fe中,形成Fe(Al)过饱和固溶体,纳米晶粉体的结构有序度较低。在1200℃,保温1h下真空热压烧结,Fe(Al)转变为有序的DO3-Fe3Al,同时发生晶粒长大。Fe3Al块体晶粒尺寸为40.1nm,相对密度大于96%,维氏硬度626.8 HV,三点弯曲强度985MPa;弯曲断口为脆性断口,但也呈现出一定韧性断裂特征。     

原位TiB2/Fe3Al基纳米复合材料的合成及其晶粒生长动力学(Ⅰ)--Fe-Al-Ti-B四元粉体的机械合金化

研究了机械合金化过程中Fe-Al-Ti-B四元粉体的结构演变,讨论了其合金化机制.研究表明,Fe-Al-Ti-B四元粉体的机械合金化通过Al、Ti、B原子向Fe晶格中扩散形成Fe（Al,Ti,B）过饱和固溶体.在机械合金化的早期（＜10h）,形成包覆结构的复合颗粒,合金化尚未进行.在机械合金化的中期（10-60h）,首先形成具有几个同心圆环结构的复合颗粒,然后环状结构消失,同时Fe（Al,Ti,B）晶格常数迅速增加,但成分均匀化过程缓慢.在机械合金化的后期（60-80h）,主要发生复合颗粒内部的成分均匀化过程,球磨80h后,复合颗粒内部各组元的成分已经非常均匀.Fe（Al,Ti,B）晶粒细小（6.8nm）,晶格畸变严重,具有近似非晶态的结构.由于Ti、B元素的添加,Fe-Al-Ti-B四元粉体晶粒细化速率更快,但合金化速率明显降低.     

反应机械合金化/退火制备Al2O3/Fe3Si纳米复合粉体

以Fe2O3粉、Si粉和Al粉为原料,采用反应机械合金化/退火法制备出了Al2O3/Fe3Si纳米复合粉体。利用X射线衍射仪（XRD）和扫描电子显微镜（SEM）对复合粉体球磨以及退火过程中的固态反应过程、表面形貌进行表征。研究表明,Fe2O3-Si-Al混合粉体球磨5 h后发生反应生成Al2 O3、Fe5 Si3、Fe3 Si、FeSi,球磨20 h后生成Al2 O3/Fe3 Si,球磨20 h的粉体在900℃条件下退火1 h的组成物相未发生变化,复合粉体颗粒呈球形,其尺寸为5μm左右,分布均匀,组成相Al2O3和Fe3Si的晶粒尺寸分别为26.6 nm和28.3 nm。     

机械合金化合成Invar合金纳米晶粉体

采用商用FeNi30及FeNi50合金粉为原料通过机械合金化(MA)合成纳米晶Invar合金(FeNi36)粉体,研究了不同球磨时间的Invar合金粉体的物相组成、显微组织结构与形貌特征,探讨其合金化机制。结果表明:球磨初期(5~10 h),微锻造和冷焊过程使合金粉体呈扁平形复合层状结构,同时FeNi50中的Ni原子逐渐向FeNi30中扩散,发生成分均匀化;球磨40 h后,已形成了成分均匀的α'-Fe(Ni)固溶体,其平均晶粒尺寸约为12 nm。此时,机械合金化合成的Invar合金粉体呈球形,表面光滑,继续球磨,大颗粒粉体表面出现裂纹,并碎裂,导致粉体细化。     

高能球磨时间对CNTs/Al5083纳米晶粉体微观组织及性能的影响

采用机械合金化法制备出2wt%CNTs/Al5083纳米晶复合粉体,研究了高能球磨时间对CNTs/Al5083纳米晶粉体性能的影响。利用XRD、SEM和TEM对该复合粉体的形貌及显微组织进行观察。结果表明,延长球磨时间可改善CNTs在Al5083粉末中的分散性,并使CNTs逐渐嵌入到金属粉末中,同时使复合粉体的晶粒细化。在球磨2.5 h时,晶粒尺寸达到46.4nm。另外,2.5h的球磨时间,会破坏CNTs的结构,同时诱发动态再结晶,使晶粒变粗,不利于粉末烧结。     

Synthesis and grain growth kinetics of in-situ FeAl matrix nanocomposites（ Ⅰ ）： Mechanical alloying of Fe-A1-Ti-B composite powder

Three nanocrystalline alloys, FesoAlso, Fe42.5Al42.5Ti5B10 and Fe35Al35Ti10B20 （molar fraction, %）, were synthesized from elemental powders by high-energy ball milling. The structural evolutions and morphological changes of the milled powders were characterized by X-ray diffractometry（XRD）, transmission electron microscopy（TEM） and scanning electron microscopy（SEM）. The effects of different Ti, B additions on the structure and phase transformation in these alloys were also discussed. It is observed that the diffusion of AI, Ti, B atoms into Fe lattice occurs during milling, leading to the formation of a BCC phase identified as Fe（Al） or Fe（Al, Ti, B） supersaturated solid solution. Fe-based solid solution with nanocrystalline structure is observed to be present as the only phase in all the alloy compositions after milling. Furthermore, the contents of Ti, B affect the formation of mechanical alloying products, changes in the lattice parameter as well as the grain size.     

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。     

Synthesis of TiB2 nanocrystalline powder by mechanical alloying

1 Introduction TiB2 has been widely used in some industrial fields owing to its high melting temperature, hardness, elastic modulus, electro-conductibility and thermal diffusivity, and excellent refractory properties and chemical inertness. Usually, TiB2…     

机械合金化制备Ti(Al,C)复合粉末组织结构研究

目的通过原位合成技术获得Ti(Al,C)复合粉末。方法在不同球磨时间条件下,采用机械合金化方法制备Ti(Al,C)复合粉末,其中Ti粉和Al粉的摩尔比为1:1。采用扫描电子显微镜(SEM)以及X-射线衍射仪(XRD)分析球磨后粉末的显微组织结构及物相,研究不同球磨时间对制备Ti(Al,C)复合粉末物相演变、组织结构及粒子间界面结合状态的影响。结果在球磨过程中,球磨时间越长,粉体的粒径越小,当球磨时间增长到一定程度时,延展性好的Al粉颗粒发生扁平化且其表面积不断增大,使得碎化后的Ti粉颗粒不断嵌入至Al粉颗粒中,最终形成Ti(Al)固溶体。同时根据XRD分析发现,随着球磨时间的延长,Ti(Al,C)复合粉末中的Al峰逐渐减小,说明Al不断固溶到Ti中,形成了一定量的Ti(Al)固溶体。结论通过机械球磨技术在球磨一定时间后可原位合成Ti(Al)固溶体,这说明随着Ti与Al之间的相互扩散,有利于形成Ti(Al)固溶体。     

机械合金化制备TiB2-Ni(Al)复合粉末组织结构研究

目的通过原位合成技术获得TiB_2-Ni(Al)复合粉末。方法采用机械合金化方法在不同球磨时间的条件下,制备不同体积含量的TiB_2陶瓷相增强Ni(Al)基复合粉末,其中Ni粉和Al粉的摩尔比为1:1。采用扫描电子显微镜(SEM)以及X-射线衍射仪(XRD)分析球磨后粉末的显微组织结构及物相,研究不同球磨时间对制备TiB_2-Ni(Al)复合粉末物相演变、组织结构及粒子间界面结合状态的影响。结果在球磨过程中,球磨时间越长,Ni/Al间的塑变有利于原子之间的扩散,TiB_2陶瓷相颗粒逐渐变小。当球磨时间增长到一定程度时,延展性好的Al粉颗粒发生扁平化且其表面积不断增大,使得碎化后的Ni粉颗粒不断嵌入Al粉颗粒中,最终形成Ni(Al)固溶体。同时根据XRD分析发现,随着球磨时间的延长,TiB_2-Ni(Al)复合粉末中的Al峰逐渐减小,说明Al不断固溶到Ni中,形成了一定量的Ni(Al)固溶体。结论通过机械球磨技术在球磨一定时间后可原位合成Ni(Al)固溶体,这说明随着Ni与Al之间的相互扩散有利于形成Ni(Al)固溶体。     

Characterization and formation mechanism of nanocrystalline (Fe,Ti)3Al intermetallic compound prepared by mechanical alloying

The nanocrystalline (Fe,Ti)₃Al intermetallic compound was synthesized by mechanical alloying (MA) of elemental powder with composition Fe₅₀Al₂₅Ti₂₅. The structural changes of powder particles during mechanical alloying were studied by X-ray diffractometry and microhardness measurements. Morphology and cross-sectional microstructure of powder particles were characterized by scanning electron microscopy. It was found that a Fe/Al/Ti layered structure was formed at the early stages of milling followed by the formation of Fe(Ti,Al) solid solution. This structure transformed to (Fe,Ti)₃Al intermetallic compound at longer milling times. Upon heat treatment of (Fe,Ti)₃Al phase the degree of DO₃ ordering was increased. The (Fe,Ti)₃Al compound exhibited high microhardness value of about 1050 Hv.     

High spatial resolution PEELS characterization of FeAl nanograins prepared by mechanical alloying

We investigate the nanograin “chemical” structure in a nanostructured material of possible industrial application (Fe–Al system) prepared by conventional mechanical alloying via ball milling in argon atmosphere. We restrict ourselves to the structural and nanochemical behaviour of ball-milled nanocrystalline Fe–Al powders with atomic composition Fe₃Al, corresponding to a well-known intermetallic compound of the Fe–Al system. Scanning transmission electron microscopy (STEM) equipped with a parallel detection electron energy loss spectrometer (PEELS) has provided an insight on the “chemical” structure of both nanograins and their surface at a spatial resolution of better than 1 nm. The energy loss near edge structure of the Al L loss reveals that the Al coordination is similar to a B2 compound and the oxidation of the powder during processing may play a significant role in the stabilization of the intermetallic phases. Conventional transmission electron microscopy (TEM) was used for the structural characterization of the material after the ball milling; powder X-ray diffraction (XRD) aided the investigation.     

The FeAl–30%TiC nanocomposite produced by mechanical alloying and hot-pressing consolidation

Intermetallic matrix composites reinforced with particles such as TiC have attracted a great deal of attention over the past few years. In the present study, the mechanical alloying process followed by hot-pressing consolidation was used to produce FeAl–30%TiC nanocomposite. Since the reduction of grain size to the nanometer scale improves mechanical properties of materials, this composite may be attractive for structural applications. An elemental powder mixture of Al35Fe35Ti15C15 (in at.%) was milled in a high-energy ball mill. The phase transformations in the powder during milling were studied with the use of X-ray diffraction (XRD). Transmission electron microscopy and differential scanning calorimetry were used for examining the microstructure and the thermal stability of the milling product. The results obtained show that high-energy ball milling as performed in this work leads to the formation of a bcc phase identified as the Fe(Al) solid solution and a fcc phase identified as TiC, and that both phases are nanocrystalline. Subsequently, the milled powder was sintered at 750 °C under pressure of 4 GPa. The XRD investigations of the consolidated pellet revealed that after sintering, the material remained nanocrystalline and that there were no phase changes, except for the ordering of Fe(Al), i.e. formation of FeAl intermetallic compound, during the sintering process. The average hardness of the obtained nanocomposite is 1287 HV_0.2 (12.6 GPa) and its density is 98% of the theoretical value.     

机械合金化Fe-40Al合金粉末工艺研究

以Fe粉、Al粉末为对象,采用机械合金化制备Fe-40Al合金复合粉末,研究球磨工艺参数对Fe-40Al合金粉末形貌及组织结构的影响规律,为机械合金化制备适合冷喷涂用Fe-40Al合金粉末提供最佳的工艺参数。研究结果表明,球磨后的Fe-40Al合金粉末具有独特的层状组织结构,随着球磨时间的延长,Fe-40Al合金粉末的平均粒径不断减小,由于Fe、Al相互扩散作用加强,粉末内部的层状结构不断细化而消失;随着球料比增加,机械合金化效率显著提高,相同球磨时间内Fe-40Al合金粉末粒径减小的幅度显著增大,同时粉末内部合金化过程加剧,导致层状结构快速消失。