机械合金化Fe－Ti合金非晶形成能力的研究

利用Ｘ光衍射和扫描电镜对机械合金化Ｆｅ－Ｔｉ非晶合金的形成过程进行了研究。试验表明，机械合金化非晶形成的过程可以分为二个阶段：粉末的破碎阶段和非晶的形成阶段。此外，对Ｆｅ－Ｔｉ合金形成非晶的成分范围进行了理论计算和试验测定。结果表明，ＦｅｘＴｉ１－ｘ可以在０．３０≤ｘ≤０．５０的范围内形成非晶，这与理论计算值基本一致。     

球磨法制备α′-Fe(N)超细粉末

通过球磨α－ Ｆｅ 和脲的混合粉末，制得α′－ Ｆｅ（Ｎ） 超细粉末．使用Ｘ 射线衍射仪（ＸＲＤ） 、透射电镜（ＴＥＭ） 和热失重（ＴＧＡ） 分析了在真空条件下经１３０ ｈ 和２００ ｈ 球磨后的粉末样品的结构和性能．结果表明，经１３０ ｈ 球磨后开始得到α′－ Ｆｅ（Ｎ） 相；热分析表明，α′－ Ｆｅ（Ｎ） 相在４３０℃以下是稳定的；经球磨２００ ｈ 后，得到α′－ Ｆｅ（Ｎ） 超细粉末（０ ．０３～０ ．０６ μｍ） ，它是ｒ（Ｎ） 为１３ ．４９％ 的过饱和固溶体．     

机械合金化Fe—Ti合金非晶形成能力的研究

利用Ｘ光衍射和扫描电镜对机械合金化Ｆｅ－Ｔｉ非晶合金的形成过程进行了研究。试验表明，机械合金化非晶形成的过程可以分为二个阶段；粉末的破碎阶段和非晶的形成阶段。此外，对Ｆｅ－Ｔｉ合金形成非晶的成分范围进行了理论计算和试验测定。     

机械合金化过程中Fe70B30粉末晶粒尺寸和微观应变的研究

用Ｘ射线和电镜研究了Ｆｅ＿（７０）Ｂ＿（３０）粉末经不同时间高能球磨后晶粒尺寸和微观应力的变化。在机械合金化过程中，粉末的Ｘ射线衍射谱的宽度随球磨时间的增加逐渐加宽，这是晶粒细化和内部微观应力共同作用的结果。Ｘ射线衍射结果表明：随着机械合金化的进行，粉末的晶粒尺寸逐渐减小，球磨初期晶粒尺寸下降较快，经１５ｈ球磨，晶粒尺寸为２５ｎｍ，机械合金化进行到一定时间后晶粒尺寸下降缓慢，８０ｈ球磨后晶粒尺寸可达５ｎｍ。在机械合金化过程中球磨所造成的微观应变不大，球磨初期粉末的内应力随球磨时间增加而增加，当粉末粒子尺寸很小时，随球磨的进行粉末中的微观应变显著下降。     

机械合金化制备Cu-Cr-C复合粉体

以Cu、Cr、C粉末为原料,采用机械合金化方法制备CuCr-C复合粉体,其中Cr、C的添加量按照Cr_3C_2质量分数为5%来计算;利用X射线衍射(XRD)和扫描电镜(SEM)研究机械合金化过程中粉末的物相和微观形貌,并结合能谱仪(EDS)面扫描得到粉末的元素微观分布。结果表明:随着机械合金化的进行,C、Cr和Cu形成Cu-Cr-C过饱和固溶体,随着球磨时间的延长,粉末粒径细化,颗粒形态由片状向球状发展;球磨30 h后,生成Cr_3C_2增强相,粉末细化趋势变缓并逐渐产生团聚,故原位生成Cr_3C_2的最佳球磨时间为30 h。     

球磨技术制备铁的氮化物及性能研究

本实验通过球磨α－Ｆｅ和脲的混合粉末,制得α’－Ｆｅ（Ｎ）超细粉末,Ｎ原子含量为８．８％（原子分数）,饱和磁化强度σｓ为２４２．７ｅｍｕ／ｇ。样品径１６０℃真空退火４ｈ,α－Ｆｅ’（Ｎ）相部分转变为α”－Ｆｅ１６Ｎ２相,此时样品的饱和磁化强度σｓ提高到２５２．０ｅｍｕ／ｇ,样品中α”－Ｆｅ１６Ｎ２相含量约２１％（质量分数）,其σｓ为２８７．０ｅｍｕ／ｇ。样分析表明,在１５０￣２００℃,α’－Ｆｅ（     

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。     

机械合金化制备高性能NdFe10.5Mo1.5Nx永磁粉

采用氩一氩等离子体电弧制备近球形或近正六边形纳米Ｎｄ、Ｆｅ、Ｍｏ粉末。以纳米Ｎｄ、Ｆｅ、Ｍｏ粉末为原料在高纯Ａｒ保护下进行机械合金化形成非晶和纳米晶α－Ｆｅ,然后在７００￣８００℃晶化２ｈ通过固态相变得到ＴｈＭｎ１２型结构的Ｎｄ、（Ｆｅ,Ｍｏ）１２,最后经４５０℃氮化２ｈ得到优异永磁性能的Ｎｄ（Ｆｅ,Ｍｏ）１２Ｎｘ粉末,Ｂｒ达０．８５￣．９８Ｔ（８．５￣９．８ｋＧｓ）,Ｈｅ达５５７．２￣７２４．４     

Fe—Mn和Fe—Mn—Si粉末混合物的机械合金化

对Ｆｅ－２４Ｍｎ，Ｆｅ－２４Ｍｎ－６Ｓｉ成分的粉末混合物进行了机械球磨，并对不同时间的球磨样品进行了Ｘ射线衍射（ＸＲＤ）和Ｍｏ¨ｓｂａｕｅｒ谱测量。结果表明，球磨使得Ｆｅ、Ｍｎ、Ｓｉ在原子尺度上发生了混合，形成了顺磁性、面心立方结构的Ｆｅ－２４Ｍｎ或Ｆｅ－２４Ｍｎ－６Ｓｉ纳米晶合金，这是Ｆｅ、Ｍｎ或Ｓｉ原子由颗粒表面到体内扩散的结果。球磨６７ｈ以后结构未发生变化，表明形成的是一种热力学亚稳结构，这个结果与Ｆｅ－Ｍｎ和Ｆｅ－Ｍｎ－Ｓｉ合金在室温下的相图结构明显不同。     

Ti—Fe二元系在机械合金化过程中的结构转变及纳米晶TiFe储氢合金的制备

研究了Ｔｉ－Ｆｅ和Ｔｉ－Ｆｅ－Ｍｎ纳米晶储氢合金的机械合金化制备，用Ｘ－ｒａｙ衍射分析了Ｔｉ－Ｆｅ和Ｔｉ－Ｆｅ－Ｍｎ在高能球磨的机械合金化过程中的结构变化及获得的ＦｅＴｉ相的晶粒尺寸。此外，还考察了球磨条件包括气氛、球磨机转速等对球磨过程中结构变化的影响。研究结果表明：采用适当的球磨参数并辅以后续热处理，可以制备出不同晶粒尺寸的纳米晶储氢合金，在本研究中获得的ＦｅＴｉ合金的最小平均晶粒尺寸可达１３ｎｍ。     

球磨时间对热压烧结制备TiC-CoCrFeNi复合材料微观组织及力学性能的影响

采用机械合金化-热压烧结法,制备TiC-CoCrFeNi复合材料,研究球磨时间对材料微观组织及力学性能的影响。结果表明:Co,Cr,Fe和Ni粉体在球磨10h后形成fcc结构的单相固溶体。经1200℃/1h热压烧结后,烧结体中生成TiC和Cr7C3结构的碳化物,并弥散分布于CoCrFeNi固溶体中。球磨时间显著改变了烧结体中碳化物的数量和尺寸,进而影响材料的力学性能。在球磨10h时,烧结体中纳米级TiC相急剧增多,此时复合材料的硬度(671HV)和屈服强度(1440MPa)达到最大值。     

Synthesis of the Supermalloy Powders by Mechanical Alloying

The mixture of the Ni, Fe and Mo elemental powders with the nominal composition of the Supermalloy was milled in a planetary mill under Ar atmosphere. Several milling times have been used ranging from 4 to 16 h. A heat treatment of 30 min, 1, 2 and 4 h at temperature of 350°C has been performed in vacuum in order to improve the alloying process and remove the internal stresses. The formation of the Fe-Ni-Mo alloys by mechanical alloying was evidenced by X-ray diffraction. The nanocrystalline Supermalloy powders have been obtained after 16 h milling and after 8 h milling followed by 4 h annealing. A typical grain size of 11 ± 2 nm have been obtained after 16 h milling. The chemical homogeneity composition and the morphology of the powder particles have been studied by X-ray microanalysis and scanning electron microscopy respectively.     

Can the degree of crystallinity of ball-milled Mg2Ni intermetallic compound decide its electrochemical characteristics?

ABSTRACT

Nanostructured Mg₂Ni intermetallic compounds were synthesized by high-energy ball milling. Effect of milling time on structure and surface morphology of milled powders were studied using x-ray diffraction and scanning electron microscopy. Crystallite size and degree of crystallinity were confirmed by using transmission electron microscopy and selected area electron diffraction analysis. The particle size of 20 h milled electrode material is 230 nm and it reduced to 40 nm when the milling time is increased to 30 h. Further increase in the milling time reduces the particles size drastically and starts agglomerating. In order to understand the effect of milling time on reaction rates, differential thermal analysis was performed. Activation energy of the milled powders was calculated using Kissinger analysis. 30 h milled powder exhibits lower activation energy than others. Cyclic voltammetry, electrochemical impedance spectroscopy, and charge–discharge studies were done on the prepared electrode materials. 30 h milled electrode material delivers maximum discharge capacity with a superior capacity retention after 20 cycles at 20 mAg^?1.     

Structure and magnetic properties of ZrO2-coated Fe powders and Fe/ZrO2 soft magnetic composites

Fe particles were coated with ZrO₂ nanopowders using mechanical milling method combined with high temperature recovery annealing process. The effect of milling time on particle size, phase structure and magnetic properties of the core-shell structure powders was studied. Scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS) and X-ray diffraction (XRD) revealed that the surfaces of the composite powders comprised thin and uniform layers of ZrO₂ insulating powders after milling. Also, the SEM images showed the morphology of micro-cellular structured compacts with cell-body of Fe particles and indicated that Fe particles were well separated and insulated by thin ZrO₂ layers. The Fe/ZrO₂ soft magnetic composites displayed much higher electrical resistivity, lower core loss than that of the pure Fe powder cores without ZrO₂ layers at medium and high frequencies. The preparation method of ZrO₂-insulated Fe powders provides a promising method to reduce the core loss and improve the magnetic properties for soft magnetic composite materials.     

Processing of nanocrystalline FeAlX (X = Ni, Mn) intermetallics using a mechanical alloying and hot pressing techniques

Fe-40Al-40Ni-20 and Fe-40Al-40Mn-20 (all in at.%) intermetallics were mechanically alloyed for 40 h and followed by hot-pressing at 650°C under 450 MPa for 1 h. As resulted from the X-ray diffraction studies, the ordered B2 structure was formed in the Fe-40Al-40Ni-20 alloy while in the case of Fe-40Al-40Mn-20 alloy, the disordered Fe(Al) solid solution was observed. The chemically homogenous rounded particles of size of about 5 μm were identified using scanning analytical electron microscopy in alloys after 40 h of milling. TEM studies of milled powders revealed a nanostructure in both alloys with grain size of about 20 nm. The hot pressing process of milled powders allowed to obtain compacts with the density of about 87 and 89% of the theoretical one for Fe-40Al-40Mn-20 and Fe-40Al-40Ni-20 alloys, respectively. The micro-hardness measurements have shown that the alloy with the Ni addition possesses the hardness of about 1200 HV₂₀, whereas in the alloy with the Mn addition it is 1100 HV₂₀. The TEM investigations allowed to identify a nanocrystalline structure of compacts with a mean grain size below 50 nm, with B2 ordered structure in both alloys.     

球磨参数对ODS奥氏体不锈钢机械合金化效果的影响

为了研究球磨参数对ODS奥氏体不锈钢机械合金化效果的影响,以Fe、Cr、Ni、W、Ti纯金属元素粉末和纳米Y2O3为原料进行混合(配比为Fe-18Cr-8Ni-2W-1Ti-0.35Y2O3,质量分数),通过高能球磨的方式实现混合粉末的机械合金化.研究球磨时间、转速的变化对粉末粒度、成分均匀度和固溶程度的影响.结果表明,在真空环境下,球料比为10∶1、转速为380r/min、球磨时间60h时,粉末达到了很好的机械合金化效果,成分分布均匀;当球磨时间延长到100h时,粉末颗粒达到最细,继续球磨,粉末将出现明显的团聚.对最优机械合金化工艺参数获得的粉末进行热压致密化研究表明,随着温度的升高,试样的密度随之升高,维氏硬度随之降低.     

Synthesis, characterization and annealing of mechanically alloyed nanostructured FeAl powder

Elemental powders of Fe and Al were mechanically alloyed using a high energy rate ball mill. A nanostructure disordered Fe(Al) solid solution was formed at an early stage. After 28 h of milling, it was found that the Fe(Al) solid solution was transformed into an ordered FeAl phase. During the entire ball milling process, the elemental phase co-existed with the alloyed phase. Ball milling was performed under toluene to minimise atmospheric contamination. Ball milled powders were subsequently annealed to induce more ordering. Phase transformation and structural changes during mechanical alloying (MEA) and subsequent annealing were investigated by X-ray diffraction (XRD). Scanning electron microscope (SEM) was employed to examine the morphology of the powders and to measure the powder particle size. Energy dispersive spectroscopy (EDS) was utilised to examine the composition of mechanically alloyed powder particles. XRD and EDS were also employed to examine the atmospheric and milling media contamination. Phase transformation at elevated temperatures was examined by differential scanning calorimeter (DSC). The crystallite size obtained after 28 h of milling time was around 18 nm. Ordering was characterised by small reduction in crystallite size while large reduction was observed during disordering. Micro hardness was influenced by Crystallite size and structural transformation.     

Magnetic properties of iron nitride-silica nanocomposite materials prepared by high-energy ball milling

Powder mixtures of (FexN)y and (SiO2)1-y, with x between 3 and 4 and y equal to 0.2 or 0.6, were ball-milled for 4, 8, 16, 32, and 64 h. X-ray diffraction, thermal analysis, and magnetization measurements allowed an investigation of structural and magnetic properties to be carried out. The samples consist of nanostructured Fe3N and Fe4N particles in a SiO2 matrix. As the milling time increases, the Fe4N phase is eliminated from the particles in favor of Fe3N. Coercive fields as high as 270 and 84 Oe are obtained for (FexN)0.2(SiO2)0.8 at 5 and 300 K, respectively. This higher coercive field, upon cooling, indicates the presence of small superparamagnetic particles. The coercive field also increases with milling time, which is due to the reduced particle size and induced stain. The saturation magnetization decreases with increased milling time as a consequence of an increase in the superparamagnetic fraction and increased strain. Hard and soft magnetic properties are observed for y = 0.2 and y = 0.6 samples, respectively.     

Effect of powder characteristics on Cr internal oxidation for preparation of Cr2O3/Cu composite

Abstract

Cr O₃/Cu composite was prepared by the internal oxidation of Cu–Cr pre-alloyed powders formed by high energy milling. Effects of milling time on the internal oxidation characteristics of Cu–Cr pre-alloyed powders were also discussed in this paper. The results indicate that the degree of the internal oxidation continually increases with prolonged milling time. At the initial stage, external oxidation rather than internal oxidation occurs, resulting in coarse Cr₂O₃ particles. With further milling, the internal oxidation becomes more complete and the sizes of Cr₂O₃ particles also become finer and well distributed. The properties of the composite are therefore improved. A high quality composite specimen from Cu–1·0Cr pre-alloyed powders after 40 h milling was prepared by the internal oxidation process. The Cr₂O₃ particles with an average size of 2–5 μm in diameter and about 5–10 μm in particles space were found by a microstructure examination, and they were uniformly dispersed in the Cu matrix.     

Effect of milling time,MWCNT content,and annealing temperature on microstructure and hardness of Fe/MWCNT nanocomposites synthesized by high-energy ball milling

Nanocrystalline pure Fe and Fe/MWCNT nanocomposites powders with 0.25, 0.5, 1, and 10 wt% MWCNT contents were synthesized by high-energy ball milling (HEBM). The as-milled powders were cold-compacted and annealed at 400 °C and 600 °C for 1 h in Ar atmosphere. The effect of ball milling on pristine MWCNT and Fe/MWCNT composite powders was also investigated as a function of milling time up to 20 h. The physical properties of MWCNT were imaged by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) before and after HEBM. The structural damage of MWCNT as a function of milling time and MWCNT content was studied using Raman spectroscopy. The structural characterization of MWCNT and Fe/MWCNT composites was conducted by X-ray diffraction (XRD) as a function of milling time, MWCNT content, and annealing temperature. The chemical properties of the synthesized composite powders were investigated using X-ray photoelectron spectroscopy (XPS). The microhardness test was performed to assess the effect of milling time, annealing temperature, and MWCNT content on the mechanical properties. The results indicated that after the ball milling process, the structure of MWCNT was destroyed, and the formation of the amorphous carbon phase was observed, which was confirmed by XRD and TEM analyses. In addition, decreased defect and carbon intensity ratios (I_D/I_G) were calculated from the Raman results with longer ball milling processes, which is attributed to the destruction of carbon bonds. The XPS results confirmed the presence of FeC bonds as a result of the formation of carbide phases. A fine dispersion of precipitated carbides determined by TEM is found to promote the grain size stability below 100 nm in the nanocrystalline Fe matrix. The results from the micro-hardness tests showed that Orowan particle strengthening resulting from the carbide formation, as well as grain size hardening, is an important contributor to strengthening in Fe/MWCNT composites.