高能球磨稀土高硅铝合金粉末性能表征

对快速凝固法制备得到的Al-20Si-0.35RE合金进行不同时间的高能球磨, 然后对球磨后的粉末进行多次热压变形, 采用XRD, ESEM以及TEM等表征变形前后合金粉末的显微组织, 并对变形后合金的导电性能进行了研究. 研究发现快速凝固Al-20Si-0.35RE合金粉末的显微组织主要由细小的Al-Si固溶体(0.3～0.5 μm)、初晶硅、稀土铝硅化合物(0.16～0.3 μm)组成; 随着球磨时间延长, 颗粒粒径显著减小; 经过多次热压变形后合金晶粒显著细化, 晶格畸变减小, 位错钉扎稀土化合物, 形成类似表面渗流效应, 合金导电率提高至70%IACS.     

高能球磨制备高铝锌铝合金粉末的研究

首先采用一步球磨法制备了成分为Zn-30Al-6Si-0.5Cu(质量分数/%)和Zn-30Al-3Si-3Cu(质量分数/%)的高铝锌铝合金粉末,其次采用二步球磨法制备了成分为Zn-30Al-6Si-0.5Cu(质量分数/%)的合金粉末,并利用XRD、SEM粒度分析仪对粉末的物相组成、颗粒形貌及粒度进行了表征和分析。结果表明:含硅量为6%的合金粉末的颗粒尺寸比含硅量为3%的合金粉末更为细小,尺寸分布更为集中,球磨12h之后的粉末其金相组织主要由富Al的α相、富Zn的η相以及Si相组成。经过二步球磨后的Zn-30Al-6Si-0.5Cu粉末中Al9Si相基本消失,Si相含量增加;二步球磨法制备的粉末颗粒尺寸更为细小。通过扫描电镜观察发现粉末形貌不规则,且分布不够均匀,粉末中基本未观察到类似焊片的颗粒。     

固溶温度对新型Al-12.7Si-0.7Mg合金挤压材组织性能的影响

针对我国自主研制的新型Al-12.7Si-0.7Mg合金挤压型材,采用金相显微镜、扫描电镜及其附带的能谱分析仪以及拉伸实验研究了固溶温度对铝基体晶粒、合金相粒子尺寸、形状及数量以及挤压材力学性能的影响规律,结果表明:Al-12.7Si-0.7Mg合金挤压材基体中存在大量尺寸极其细小的点状Mg2Si相及大量微米级共晶Si粒子和少量微米级AlFeSi过剩结晶相;固溶温度从440℃升高至540℃,尺寸极其细小的点状Mg2Si相逐渐回溶入基体消失,微米级共晶Si颗粒及含AlFeSi的过剩结晶相粒子形状趋于球化,而铝基体晶粒呈现出略有长大的趋势,且共晶硅颗粒具有较明显的细化铝基体晶粒的作用;合金挤压材的强度及延伸率随固溶温度升高分别呈现出单调增大及总体下降的趋势;新型Al-12.7Si-0.7Mg合金挤压材比较适宜的固溶温度为520℃,合金挤压材经最佳固溶温度固溶水淬再经170℃×2.5 h时效处理后的Rp0.2≥279 MPa,Rm≥330 MPa,A≥9.9%。     

氮化物弥散强化铁基合金的显微组织和力学性能研究

本实验向雾化Fe-12.8Cr-3.4W铁基粉末中引入氮化物粉末进行球磨,然后对球磨粉末进行热挤压和热轧制制备得到合金样品。对雾化粉末和球磨粉末的形貌和成分、各组成形合金的显微组织、各组成形合金的力学性能以及断口形貌进行了研究。实验结果表明,球磨对粉末晶粒起到了细化作用,同时球磨后粉末与空气接触会引入少量的氧,YN(氮化钇)的引入起到了细化球磨粉末的作用;在氮化物弥散强化合金中检测到了尺寸小于100 nm的Ti N和TiO_2的复合弥散颗粒,少量弥散颗粒与合金中的Cr、W、Y和O元素结合长大形成大于100 nm的复杂化合物颗粒。采用氮化钇制备的合金抗拉强度与氧化钇合金基本相同,延伸率增加,同时显微硬度提高;采用氮化钛和氮化钇进行制备的合金显微硬度进一步增加。     

高能球磨制备Zr-V纳米粉末

将初始Zr粉和V粉按一定比例混合 ,用高能球磨设备制备Zr V纳米粉末 ,利用XRD和SEM及TEM研究研磨过程中粉末的物相及粒度变化。结果表明 ,粉末的晶粒尺寸随研磨时间的增加而减少 ,适当增加转速 ,可以缩短晶粒细化时间 ;通过高能球磨可以制备出粉末晶粒尺寸在 10nm左右 ,粉末颗粒尺寸在 6nm左右的Zr V混合粉末     

高能球磨-放电等离子烧结法制备双晶分布钛

以平均粒径约150μm的球形钛粉为原料,采用高能球磨结合放电等离子烧结技术制备由双尺度晶粒组成的高致密纯钛块体材料,研究高能球磨过程中钛粉的形貌、尺寸及显微组织的变化,分析球磨钛粉放电等离子烧结时的致密化行为和显微组织的演变规律,测试烧结钛块体材料的室温压缩性能。结果表明:钛粉在球磨初期发生剧烈的塑性变形并相互焊合,形成层片状团聚粉末。球磨10 h时,钛粉的部分晶粒细化至40~100 nm。放电等离子烧结过程中,随烧结温度升高和烧结时间延长,烧结钛的密度逐渐增大。在烧结温度为800℃、保温时间为4 min、烧结压力为50 MPa的条件下,烧结钛的密度达到4.489 g/cm3,接近全致密,其显微组织由双尺度的等轴晶组成,细晶区晶粒尺寸为1~2μm,粗晶区晶粒尺寸为5~20μm,二者呈层状交替分布;该试样在室温压缩条件下的综合力学性能与铸锻Ti-6Al-4V合金相当。     

机械合金化制备纳米晶Fe-Si合金的研究

采用Fe-6．5％Si合金粉与Si-22％Fe合金粉末，经机械合金化制备了Fe-13．95％Si固溶体合金。由碰撞频率、速率与球磨工艺条件的理论关系推导出了球料比的最佳值。利用XRD、SEM和EDX手段对球磨后的Fe—Si粉体进行了结构、形貌及成份表征。结果表明：混合粉体球磨12h可实现机械合金化，合金化的粉体为α—Fe（Si）过饱和固溶体，颗粒尺寸为0．5～15μm，显微组织为纳米晶结构，平均晶粒尺寸约为18nm。     

球磨时间对Al2O3/Mo复合材料组织与性能的影响

采用溶胶-凝胶法制备Al2O3/Mo混合粉体,利用高能球磨法细化Al2O3/Mo复合材料中氧化铝和钼的晶粒尺寸,研究了球磨时间对Al2O3/Mo复合材料组织与性能的影响,利用XRD和扫描电镜对复合粉末形貌和复合材料进行了物相和形貌分析。研究表明:随着球磨时间的延长,复合粉末的形貌经历了球状到层片状再到球状的变化,粉末粒度逐渐减小,经粉末冶金烧结后的复合材料中,氧化铝和钼的粒径逐渐减小,经过60h的球磨,氧化铝颗粒的尺寸达到500nm左右;复合材料的密度呈现先增加后减小的趋势,显微硬度则逐渐上升至403.2HV。     

Mo-Si-B基超高温合金粉体的机械合金化

采用XRD,SEM和EPMA等方法分析Mo-12Si-10B-3Zr-0.3Y(原子分数)混合粉末在500 r/min转速下进行球磨时的机械合金化行为。结果表明:球磨后在混合粉末中并未形成Mo3Si和Mo5SiB2化合物相,而仅形成了合金元素在Mo中的过饱和固溶体Moss和弥散分布于其中的亚微米级B颗粒。随球磨时间延长,Moss的晶粒尺寸不断减小,其微观应变不断增加,球磨30 h后两者分别约为47 nm和0.53%;从XRD谱可知,球磨2 h后有少量的α-MoSi2生成,但球磨30 h后其衍射峰消失。球磨5 h后混合粉末由层片状的复合颗粒组成,球磨10 h后层片状复合颗粒破裂并转变为等轴状,球磨30 h后混合粉末由平均粒径约1μm的球状团聚体颗粒组成。     

机械合金化诱导难互溶系Cu-Cr合金固溶度扩展的研究

采用机械合金化工艺制备Cu-4%Cr和Cu-7%Cr(原子分数)二元合金粉末,利用XRD,SEM和TEM研究机械合金化过程中粉末的微观形貌和显微组织结构,测量了不同球磨时间粉末的氧含量以及显微硬度.结果表明:在一定的球磨时间内,Cu-Cr合金粉末随着高能球磨的进行,晶粒逐渐细化至纳米尺寸,晶格畸变增加,但进一步球磨会导致铜的晶格常数有所增加,畸变降低.实验证明,在固态下几乎不互溶的Cu-Cr合金,经球磨40 h的机械合金化,Cr在Cu中的固溶度明显提高.     

粉末冶金制备的Ti35Nb2．5Sn5HA生物复合材料的组织与性能研究

采用高能机械球磨和脉冲电流活化烧结方法制备了一种新型的不含Al、V等有毒元素的口钛合金基体的Ti35Nb2．5Sn5HA生物复合材料。研究了不同机械球磨时间球磨的Ti35Nb2．5Sn5HA粉末以及用这几种粉末烧结制备的样品微观组织和显微硬度变化,球磨时间对烧结复合材料的微观组织和性能的影响。结果表明：随着球磨时间的增加,Ti35Nb2．5Sn5HA粉末的颗粒尺寸逐渐减小,Nh和Sn开始与Ti发生固溶,形成Ti的过饱和固溶体,而且α-Ti也开始向β-Ti转化。当球磨时间达到12h,球磨粉末中α-Ti完全转化为β-Ti,粉末颗粒的平均尺寸为500nm左右。12h球磨的粉末烧结制备的复合材料具有超细晶粒尺寸,晶粒平均尺寸为200nm,这种复合材料的维氏显微硬度可以达到10187．3MPa。     

球磨时间对钨粉粒度分布及形貌影响

通过改变球磨时间,获得不同粒度分布的钨粉颗粒,分析球磨时间对钨粉粒度分布和形貌特征的影响,提高粒度分布在目标区间（5～11 μm）的钨粉颗粒体积分数。结果表明,球磨的前2 h对原料中大颗粒钨粉的影响较大,钨粉颗粒最大粒径由134 μm迅速下降到20 μm左右。随着球磨时间的增加,钨粉粒度分布指标减缓下降,除粒径变小外,颗粒形貌基本无变化,但是在球磨10 h后开始出现团聚现象。综合分析可知,球磨时间的改变对钨粉粒度分布指标影响较大,球磨时间为8 h时,可获得粒度分布最窄的钨粉颗粒,在目标区间的钨粉颗粒体积分数达到75%。     

两种高能球磨机制备Fe-Si合金磁粉的对比

分别采用行星球磨机和振动球磨机制备了Fe-6.5%Si合金磁粉.讨论了球磨时间、球料比、干、湿磨等因素对颗粒细化的影响.结果表明:颗粒尺寸随球磨时间的增加而减小,湿磨可缩短球磨时间、提高球磨效率;同等条件下,振动机的球磨效率大于行星球磨机的球磨效率.     

Ti-Y2O3 Composites with Nanocrystalline and Microcrystalline Matrix

Mechanical milling of a Ti-2 pct Y₂O₃ powders mixture led to the synthesizing of a composite powder with a nanocrystalline Ti matrix having a mean crystallite size of 19 nm. Both the nanocomposite powder prepared through milling and the initial mixture of powders were consolidated by hot pressing under the pressure of 7.7 GPa at the temperature of 1273 K (1000 °C). The transmission electron microscopy (TEM) investigations of the bulk sample produced from milled powder revealed that Y₂O₃ equiaxial particles of less than 30 nm in size are distributed uniformly in the Ti matrix with a grain size in the wide range from 50 nm to 200 nm. The microhardness of the produced nanocrystalline material is 655 HV0.2, and it significantly exceeds the hardness of the microcrystalline material (the consolidated initial mixture of powders), which is equal to 273 HV0.2. This finding confirms that reducing the grain size to the nanometric level can have a beneficial influence on the hardness of titanium alloys. Dispersion hardening also contributes to the hardness increase.     

Fabrication of ultrafine and nanocrystalline WC–Co mixtures by planetary milling and subsequent consolidations

Abstract

In this work ultrafine and nanocrystalline WC–Co mixtures were obtained by low energy milling in planetary ball mill. The effect of the processing conditions on the reduction and distribution of the grain sizes and the internal strains level were studied. The characterisation of the powder mixtures was performed by means of scanning and transmission electron microscopy and X-ray diffraction analysis. Observations through SEM and TEM images showed a particle size below 100 nm, after milling. The X-ray diffraction profile analysis revealed a WC phase refined to a crystallite size of 19 nm.

The mixtures obtained have been consolidated and mechanical and microstructurally characterised. The results show improvements in resistant behaviour of the material consolidated from nanocrystalline powders, in spite of the grain growth experienced during the sintering. The best results were found for the material obtained by wet milling during 100 h, which presents values of hardness higher than 1800 HV.     

原位合成SiC对铝基复合材料微观组织和力学性能的影响

以铝粉、硅粉、石墨粉为原料, 通过冷压真空烧结原位合成了含不同质量分数SiC颗粒的SiC/Al-18Si复合材料。利用X射线衍射仪, 扫描电子显微镜和能谱分析仪等设备手段表征了铝基复合材料的相组成和微观结构, 研究了原位合成SiC对复合材料微观结构、抗弯强度和显微硬度的影响, 分析了复合材料力学性能的变化规律。结果表明: 复合材料的基体相为Al相, 第二相为Si相和SiC相; 原位合成的SiC颗粒弥散细小的分布在Al基体中, 其颗粒尺寸主要分布在0.2~2.8 μm, 具有亚微米、微米级的多尺度特性; 随着SiC质量分数的不断增加, 复合材料的显微硬度增大, 同时颗粒的平均尺寸仅由0.81 μm增大到1.13 μm, 但仍均匀分布, 正是这种尺寸稳定性, 使得SiC/Al-18Si复合材料硬度远大于Al-18Si; 当SiC质量分数为30%时, 材料的显微硬度最高, 达到HV 134, 相较于Al-18Si提高了88%。     

球磨工艺对Al2O3/Mo复合材料组织的影响

针对原位自生Al2O3增强钼基复合材料晶粒较大的问题,采用溶胶-凝胶与高能球磨相结合的方法细化复合材料晶粒,并利用SEM、XRD对不同球磨工艺所制备Al2O3/Mo复合粉末及复合材料的组织进行了观察和分析。结果表明:随着球磨时间的延长,Al2O3/Mo复合粉末颗粒由球状变为层片状再成为细小的球状,颗粒大小由约1.5μm细化为约500nm,其中的钼晶粒不断细化;高球料比所得粉末的分散性和破碎细化程度较好;转速提高使得粉末颗粒的尺寸均匀程度降低,且伴有结块现象,不利于粉末的细化。在球料比5∶1、转速300r/min、球磨时间60h条件下获得的复合粉末,经压坯烧结可制备出Al2O3颗粒为纳米级的钼基复合材料。     

Phase transformation,structural evolution and mechanical property of nanostructured FeAl as a result of mechanical alloying

Objective of the work was to synthesize nanostructured FeAl alloy powder by mechanical alloying (MEA). The work concentrated on synthesis, characterization, structural and mechanical properties of the alloy. Nanostructured FeAl intermetallics were prepared directly by MEA in a high energy rate ball mill. Milling was performed under toluene solution to avoid contamination from the milling media and atmosphere. Mixtures of elemental Fe and Al were progressively transformed into a partially disordered solid solution with an average composition of Fe—50 at % Al. Phase transformation, structural changes, morphology, particle size measurement and chemical composition during MEA were investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Energy dispersive X-ray spectroscopy (EDS) respectively. Vickers micro hardness (VMH) indentation tests were performed on the powders. XRD and SEM studies revealed the alloying of elemental powders as well as transition to nanostructured alloy, crystallite size of 18 nm was obtained after 28 hours of milling. Expansion/contraction in lattice parameter accompanied by reduction in crystallite size occurs during transition to nanostructured alloy. Longer milling duration introduces ordering in the alloyed powders as proved by the presence of superlattice reflection. Elemental and alloyed phase coexist while hardness increased during MEA.     

Synthesis and characterisation of quasicrystalline Al based composites

Abstract

Al matrix composites reinforced by Al–Cu–Fe quasicrystalline (QC) phase particles were produced from a mixture of Al and QC powders using electrical current heating and conventional sintering. A combination of X-ray diffractrometry, transmission and scanning electron microscopy was used to characterise the microstructure of consolidated specimens. The metallic bonding of the Al matrix and particles was improved by higher temperature sintering or electrical current heating. However, the dissolution of QC particles into the Al matrix was inevitable during heating and resulted in the formation of ω and/or β phases. The dissolution of QC particles was effectively reduced using prealloyed Al powder containing 2 at.-%Cu. This had led to an increase in microhardness from 96 to 139 HV for specimens using pure Al to prealloyed Al powders. A homogeneous distribution of QC particles within the Al matrix could be achieved by mechanical milling followed by consolidation.     

Synthesis of nanosized WC/MgO powders by high energy ball milling and analysis of reaction thermodynamics

Abstract

In the present work, a powder mixture of pure WO₃, graphite and Mg with a definite atomic ratio was milled at room temperature using a high energy ball mill method, and ball milled powders were analysed by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results indicated that after ball milling for a period of time, an oxidation–reduction reaction was successfully achieved among the Mg, graphite and WO₃ powders to obtain MgO and WC. The extension of the ball milling led to the refinement of the powders. After ball milling 50 h, nanocrystalline WC grains (25 nm) were embedded into the fine matrix of MgO and formed fine nanocomposite MgO/WC powders (～100 nm in diameter). The experimental results and thermodynamic analysis showed that the formation of nanocomposite MgO/WC was a mechanically induced self-propagating reaction, and very short milling time was needed to complete the reaction.