Structural, microstructural and magnetic properties of amorphous/nanocrystalline Ni63Fe13Mo4Nb20 powders prepared by mechanical alloying

This paper focuses on the magnetic, structural and microstructural studies of amorphous/nanocrystalline Ni₆₃Fe₁₃Mo₄Nb₂₀ powders prepared by mechanical alloying. The ball-milling of Ni, Fe, Mo and Nb powders leads to alloying the element powders, the nanocrystalline and an amorphization matrix with Mo element up to 120 h followed by the strain and thermal-induced nucleation of a single nanocrystalline Ni-based phase from the amorphous matrix at 190 h. The results showed that the saturation magnetization decreases as a result of the electronic interactions between magnetic and non-magnetic elements and finally increases by the partial crystallization of the amorphous matrix. The coercive force increases as the milling time increases and finally decreases due to sub-grains formation.     

机械合金化W-Ni-Fe纳米复合粉的制备及结构研究

W,Ni,Fe粉末按照91.16W6．56Ni2.26Fe和95W5Ni的成分配比进行了机械合金化(MA)．通过调整球磨转速、球磨时间等工艺参数研究了其对粉末结构的影响,并对机械合金化粉末的物相、合金化特性、晶粒尺寸、点阵畸变及粉末形貌和颗粒度作了测定和分析讨论.机械合金化使晶粒细化并产生孪晶和位错．有利于原子扩散形成过饱和固溶体和非晶；高的球磨能有利于形成非晶相、晶粒细化和点阵畸变，350r／min球磨20h后晶粒尺寸可达25nm；输入的球磨能不同．粉末粒度的变化路径不同，但都会经历长大，变小和稳定三个不同阶段.     

Microstructural, thermal and magnetic properties of amorphous/nanocrystalline FeCrMnN alloys prepared by mechanical alloying and subsequent heat treatment

Amorphous FeCrMnN alloys were synthesized by mechanical alloying (MA) of the elemental powder mixtures under a nitrogen gas atmosphere. The phase identification and structural properties, morphological evolution, thermal behavior and magnetic properties of the mechanically alloyed powders were evaluated by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and vibrating sample magnetometer (VSM), respectively. According to the results, at the low milling times the structure consists of the nanocrystalline ferrite and austenite phases. By progression of the MA process, the quantity and homogeneity of the amorphous phase increase. At sufficiently high milling times (>120 h), the XRD pattern becomes halo, indicating complete amorphization. The results also show that the amorphous powders exhibit a wide supercooled liquid region. The crystallization of the amorphous phase occurs during the heating cycle in the DSC equipment and the amorphous phase is transformed into the crystalline compounds containing ferrite, CrN and Cr₂N. The magnetic studies reveal that the magnetic coercivity increases and then decreases. Also, the saturation magnetization decreases with the milling time and after the completion of the amorphization process (>120 h), the material shows a paramagnetic behavior. Although the magnetic behavior does not considerably change by heating the amorphous powders up to the crystallization temperature via DSC equipment, the material depicts a considerable saturation magnetization after the transformation of the amorphous phase to the nanocrystalline compounds.     

Magnetic and structural studies of mechanically alloyed (Fe50Co50)62Nb8B30 powder mixtures

Amorphous (Fe₅₀Co₅₀)₆₂Nb₈B₃₀ powder mixture was prepared by mechanical alloying from elemental Fe, Co, B and Nb powders in a planetary ball mill under argon atmosphere. Structural, thermal and magnetic properties were performed on the milled powders by means of X-ray diffraction, differential scanning calorimetry and magnetic measurements. The amorphous state is reached after 125 h of milling. The excess enthalpy due to the high density of defects is released at temperature below 300 °C. Crystallisation and growth of crystal domains are the dominating processes at high temperatures. The saturation magnetisation decreases rapidly during the first 25 h of milling to about 15.24 A m²/kg and remains nearly constant on further milling. Coercivity, H_c, value of about 160 Oe is obtained after 125 h of milling.     

合金元素对单相渗碳体磁性粉体制备及性能的影响

通过机械合金化和真空退火热处理的方法制备了单相渗碳体粉末,并结合第一性原理计算,分析了Mn、Cr和Si对合金渗碳体的成相能力及渗碳体磁学性能的影响。结果表明,机械合金化+600℃真空热处理可获得单相渗碳体。Si的加入完全抑制了渗碳体的生成,而加入Mn、Cr对渗碳体生成有促进作用。Cr、Mn合金化的渗碳体的粉末饱和磁化强度及矫顽力较未合金化时纯Fe_3C均有所降低,且Cr元素导致的降低幅度更大。合金渗碳体中Cr-C,Mn-C,Fe-C化学键合强度依次减弱,Cr、Mn合金化渗碳体的结构稳定性优于纯Fe3C。     

合金元素对Laves相增强Nb基合金的相组成

采用机械合金化与热压烧结工艺制备了添加合金元素V和Fe的Laves相增强的Nb基复合材料。研究了添加质量分数4%V和Fe的Nb/NbCr2-4.0V和Nb/NbCr2-4.0Fe配比成分的元素粉,经MA20h后在1250℃热压30min所获得的Nb/NbCr2合金的组织和性能。结果表明:在热压过程中原位合成出细小弥散分布的三元Laves相Nb(Cr,V)2和Nb(Cr,Fe)2,并且V和Fe原子只占据Laves相中的Cr原子位置。制备出的Laves相增强Nb基合金接近全致密,组织细小均匀,晶粒尺寸小于500nm。Nb/NbCr2-4.0V和Nb/NbCr2-4.0Fe合金的断裂韧性分别达到5.3和6.3MPa·m1/2,其中Nb/NbCr2-4.0Fe合金不仅抗压强度达到2256MPa,其屈服强度和塑性应变也分别达到2094MPa和6.03%。     

Structure, hyperfine interactions and magnetization studies of mechanically alloyed Fe50Ge50 and Fe62Ge38

X-ray diffraction, Mössbauer spectroscopy and magnetization measurements were used to study the structure and some magnetic properties of Fe₅₀Ge₅₀ and Fe₆₂Ge₃₈ prepared by mechanical alloying from the elemental powders. In both cases in the early stages of milling the intermediate paramagnetic FeGe₂ phase was formed. The mechanical alloying process of Fe₅₀Ge₅₀ resulted in the formation of the paramagnetic FeGe (B20) phase with an average crystallite size of about 15 nm. In the case of the Fe₆₂Ge₃₈, the ferromagnetic Fe₅Ge₃ (β) phase with a Curie temperature of about 430 K was obtained. The average crystallite size was about 9 nm. The average hyperfine magnetic field of about 16 T allowed it to determine that more than four germanium atoms exist in the nearest environment of the ⁵⁷Fe isotopes in the Fe₅Ge₃ phase.     

Kinetics and formation mechanism of amorphous Fe52Nb48 alloy powder fabricated by mechanical alloying

A single phase amorphous Fe₅₂Nb₄₈ alloy has been synthesized through a solid state interdiffusion of pure polycrystalline Fe and Nb powders at room temperature, using a high-energy ball-milling technique. The mechanisms of metallic glass formation and competing crystallization processes in the mechanically deformed composite powders have been investigated by means of X-ray diffraction, Mössbauer spectroscopy, differential thermal analysis, scanning electron microscopy and transmission electron microscopy. The numerous intimate layered composite particles of the diffusion couples that formed during the first and intermediate stages of milling time (0–56 ks), are intermixed to form amorphous phase(s) upon heating to about 625 K by so-called thermally assisted solid state amorphization, TASSA. The amorphization heat of formation for binary system via the TASSA, ΔH_a, was measured directly as a function of the milling time. Comparable with the TASSA, homogeneous amorphous alloys were fabricated directly without heating the composite multilayered particles upon milling these particles for longer milling time (86 ks–144 ks). The amorphization reaction here is attributed to the mechanical driven solid state amorphization. This single amorphous phase transforms into an order phase (μ phase) upon heating at 1088 K (crystallization temperature, T_x) with enthalpy change of crystallization, ΔH_x, of −8.3 kJ mol⁻¹.     

Fabrication of Ti-Cu-Ni-Al amorphous alloys by mechanical alloying and mechanical milling

Ti-based amorphous alloy powders were synthesized by the mechanical alloying (MA) of pure elements and the mechanical milling (MM) of intermetallic compounds. The amorphous alloy powders were examined by X-ray diffraction (XRD), differential scanning calorimetry (DSC), and scanning electron microscopy (SEM). Scanning electron micrographs revealed that the vein morphology of these alloy powders shows deformation during the milling. The energy-dispersive X-ray spectral maps confirm that each constituent is uniformly dispersed, including Fe and Cr. The XRD and DSC results showed that the milling time required for amorphization for the MA of pure elements was longer than that of the MM for intermetallic compounds. The activation energy and crystallization temperature of the MA powder are different from those of the MM powder.     

Microstructural control of and mechanical properties of mechanically alloyed tungsten heavy alloys

93W-5.6Ni-l.4Fe tungsten heavy alloys with controlled microstructures were fabricated by mechanically alloying of elemental powders of tungsten, nickel and iron by two different process routes. One was the full mechanical alloying of blended powders with a composition of 93W-5.6Ni-l.4Fe, and the other was the partial mechanical alloying of blended powders with a composition of 30W-56Ni-14Fe followed by blending with tungsten powders to form a final composition of 93W-5.6Ni-l.4Fe. The raw powders were consolidated by die compaction followed by solid state sintering at 1300°C for 1 hour in a hydrogen atmosphere. The solid state sintered tungsten heavy alloys were subsequently liquid phase sintered at 1445∼1485°C for 4-90 min. The two-step sintered tungsten heavy alloy using mechanically alloyed 93W-5.6Ni-l.4Fe powders showed tungsten particles of about 6-15 μm much finer than those of 40 um in a conventional liquid phase sintered tungsten heavy alloy. An inhomogeneous distribution of the solid solution matrix phase was obtained in the two-step sintered tungsten heavy alloy using partially mechanically alloyed powders. The two-step sintered tungsten heavy alloy using mechanically alloyed 93W-5.6Ni-l.4Fe powders showed larger elongation of 16% than that of 1% in the solid state sintered tungsten heavy alloy due to the increase in matrix volume fraction and decrease in W/W contiguity. Dynamic torsional tests of the two-step sintered tungsten heavy alloys showed reduced shear strain at maximum shear stress than did the sintered tungsten heavy alloys using the conventional liquid phase sintering.     

Progress of solid-state reaction and glass formation in mechanically alloyed Zr65Al7.5Cu17.5Ni10

The progress of amorphization in mechanically alloyed Zr₆₅Al_7.5Cu_17.5Ni₁₀ powder was investigated in detail using x-ray diffraction, Rietveld analysis, magnetic measurements, metallography, as well as scanning and transmission electron microscopy. For this purpose mixtures of elemental powders were used as starting materials and milled for distinct periods of time. Detailed investigations of the microstructural evolution during milling indicate that the amorphization proceeds by solid-state reaction, similar to what is known for mechanical alloying of binary alloy systems and other multicomponent alloys. A layered structure typical for mechanically alloyed material arises in the early stages. Alloying of the lamellae, which consist of pure elements, proceeds to some extent via anomalous fast diffusion of small-sized atoms. Besides this, the larger atoms also contribute to alloying. The observed reaction paths are compared with well-known models describing the amorphization by solid-state reaction in binary systems, suggesting that dislocation pipe diffusion plays a decisive role for intermixing the elements and promoting amorphization.     

Sintering of a nano-crystalline tungsten heavy alloy powder

A nano-crystalline Tungsten heavy alloy powder was obtained by mechanical alloying of elemental powders in a jar mill with a high ball to powder ratio. The chemical composition of the primary powder was 93 W-4.9Ni-2.1Fe (wt%). The mechanically alloyed powder had 22 nm sized tungsten crystallites distributed in an amorphous nickel base phase. Mechanical alloying reduced particle size of powders and also yielded to more uniform particles size distribution. Sintering behavior and microstructural development of that powder were studied and compared with a conventionally mixed powder. Mechanically stored energy and better distribution of primary elements in Nano-crystalline powder had decreased motivation energy of sintering and that powders showed more densification at relatively lower sintering temperatures. Sintering at low temperatures can depress grain growth during sintering and provide desirable properties. A transient intermetallic phase was formed in the nano-crystalline powder during sintering that has not been seen in conventionally mixed powders.     

机械合金化法制备Al80Fe20非晶合金形成过程的研究

用机械合金化法将晶态Al,Fe金属粉末制成了一般急冷法得不到的Al_(80)Fe_(20)非晶合金粉末,利用X衍射分析、Mossbauer谱研究了球磨非晶化的进程,用DSC研究了形成非晶的热行为。结果表明非晶化的速率受界面扩散反应控制,并随球磨时间的增加而变化,同时还考察了不同球磨条件对非晶形成的影响。     

W-Ni-Fe系机械合金化过程中的相变及热力学和动力学研究

W,Ni,Fe粉末按照91.16W6.56Ni2.28Fe的成分配比进行机械合金化(MA)。用XRD确定物相,用TEM(JEM-2000CX型)观察微观形貌和显微结构。并对机械合金化粉末的物相、颗粒尺寸、晶格畸变作了分析讨论。MA可以使W-Ni-Fe系形成纳米晶超饱和固溶体和非晶。参照Miedema半经验理论模型,计算了该合金系的相变驱动力,热力学分析指出该合金系不存在发生非晶化反应的化学驱动力。应用固态反应模型解释了MA过程非晶形成的热力学可能性,在MA过程中,非晶的形成并不绝对要求体系ΔHmix<<0和DB>>DA     

Fabrication of mechanically alloyed Ti-Ni-Cu powders and damping properties of Al/Ti-Ni-cu sintered materials

The microstructure and phase transformation of mechanically alloyed Ti-(50-x)Ni-xCu powders added to an aluminium matrix to enhance their damping properties were studied. Four compositions between 5 and 20 at.%Cu intermetallic compounds were selected to control the fraction of the martensite phase of Ti-Ni-Cu. Mechanically alloyed Ti-Ni-Cu powders were heat-treated in a vacuum of 10⁶ torr for crystallization. Mechanically alloyed Ti-Ni-Cu powders were milled with Al, swaged at room temperature and rolled at 450°C. After mechanical alloying for 10 hours. The Ti, Ni and Cu elements were completely alloyed and an amorphous phase was formed. The amorphous phase was crystallized to martensite (B19’) and austenite (B2) after heat treatment for 1 hour at a temperature of 850°C, and a Fe₂Ti intermetallic compound was partially formed. As the Cu contents increased the austenite phase fraction increased. The specific damping capacity (SDC) of Al/TiNiCu composite was higher than that of the Al/TiNi composite or native aluminium.     

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)。     

Ti—Fe机械合金化中氢致非晶化的研究

研究了氢原子对Ｔｉ－Ｆｅ系机械合金化的影响,应用 ＸＲＤ,ＤＳＣ,ＴＥＭ等方法测试了Ｔｉ－Ｆｅ系和Ｔｉ－Ｆｅ－ＴｉＨ２系的机械合金化反应过程和产物结构的特征。研究结果表明,氢原子在机械合金化过程中诱导非晶ＴｉＦｅ相的形成,由于氢原子的影响,非晶ＴｉＦｅ相的结构弛豫温度和晶化温度低于机械合金化得到的非晶ＴｉＦｅ相相应的温度。     

Formation of crystalline and amorphous solid solutions of W–Ni–Fe powder during mechanical alloying

The tungsten heavy alloy with the composition of 76.6W–17.3Ni–6.1Fe in atom percent was mechanically alloyed (MA) from the elemental powders of W, Ni and Fe. Nanocrystalline supersaturated solid solutions and amorphous phase were obtained during MA. Phase evolution, grain size and lattice distortion of these powders were determined and discussed. A thermodynamic model was developed based on semi-experimental theory of Miedema to calculate the driving force for phase evolution. The thermodynamic analysis showed that there is no chemical driving force to form the solid solution and the amorphous phase. The effect of the work of milling on the amorphization during MA was discussed and the model of multilayer amorphization during MA was applied to illustrate the feasibility of amorphization of powder with neither ΔH_mix0 nor D_BD_A. The driving force for amorphization is provided not by the negative heat of mixing or the stored energy in the grain boundaries but by the sharp concentration gradients in this system. Amorphization is mechanically driven and not by the negative heat of mixing. Crystallization is suppressed by sharp concentration gradients.     

机械合金化法制备Fe—Ni—P—B磁性非晶合金的研究

用机械合金化法研究制备Ｆｅ－Ｎｉ－Ｐ－Ｂ系磁性非晶材料,用Ｘ射线衍射仪,扫描电子显微术和透射电子显微术对不同球磨工艺处理的Ｆｅ４０Ｎｉ４０Ｐ１４Ｂ６成分的粉末进行了分析,结果表明,成分为Ｆｅ４０Ｎｉ４０Ｐ１４Ｂ６的粉末,可通过机械合金化使其非晶化。     

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…