Synthesis and characterization of Zn/Al2O3 nanocomposite by mechanical alloying

In this study, fabrication and characterization of zinc-based metal matrix nanocomposite reinforced by Al₂O₃ particles was investigated. Aluminum and zinc oxide powder mixture was milled in a planetary ball mill in order to produce Zn/Al₂O₃ nanocomposite. The structural evaluation milled and annealed powders studied by X-ray diffraction, SEM observation and hardness measurement. The zinc crystallite size estimated with broadening of XRD peaks by Williamson-Hall formula. The zinc oxide was found to react with Al through a rapid self-sustaining combustion reaction process. As a result a zinc matrix composite reinforced by Al₂O₃ particulate was formed. The microhardness value of produced nanocomposite powder was about 350 HV which was 10–15 times higher than the microhardness of pure zinc (20–30 HV).     

Synthesis and characterization of nanocrystalline Mg2CoH5 obtained by mechanical alloying

The stoichiometric mixture of 2MgH₂ + Co was ball milled under a hydrogen atmosphere to synthesize nanocrystalline metal hydride Mg₂CoH₅. Upon milling, the mixture was analyzed by X-ray powder diffraction (XRD) and thermal methods employing the techniques of differential scanning calorimetry (DSC), thermogravimetry (TG) and differential thermal analysis (DTA). Hydrogen absorption and desorption measured by pressure-composition-temperature (P-C-T) curves indicated that the capacity loss was small after 20 consecutive cycling tests. The enthalpies associated with hydride formation and decomposition were measured to be –69.5 and –83.2 kJ mol^–1 H₂, respectively. At the temperatures of this study (553 to 653 K), hysteresis decreases with increasing temperature.     

Synthesis of metastable NiGe2 by mechanical alloying

Mechanical alloying of Ni–Ge elemental powder blends was carried out in a high-energy SPEX shaker mill to study phase evolution as a function of milling time. X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy techniques were employed to characterize the phases present in the milled powders. It was noted that a supersaturated solid solution formed in the early stages of milling containing up to about 12 at.% Ge. On continued milling, the equilibrium NiGe phase started to form at 5 h, and its amount in the powder increased with increasing milling time. On milling for about 60 h, the equilibrium intermetallic NiGe and Ge powder particles reacted to form the metastable NiGe₂ phase. Reasons for the formation of this metastable phase at room temperature and at atmospheric pressure, which is normally present at high temperatures and under high pressures, have been discussed.     

Synthesis and characterization of the novel nanostructured NiC carbide obtained by mechanical alloying

In the present work, a comprehensive study of mechanical alloying of Ni-carbon nanotubes (CNT) and Ni-Graphite equiatomic powder mixtures under the same technological modes has provided to reveal the features of using different types of carbon (CNT or graphite) as a charge component. The as-milled powders were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and magnetometric study. A novel nanoscale fcc NiC monocarbide was synthesized regardless the type of the charge used. According to the XRD study the formation of this phase takes place in two stages. A two-step carbide formation mechanism has been proposed. The associated changes in the nickel lattice, such as changes in the lattice parameter, lattice strain and residual stresses, which led to the formation of NiC monocarbide were also evaluated and discussed. Parameters of the electronic structure of NiC were calculated using the MStudio MindLab 7.0 software package with the experimental data on the crystal structure of the NiC phase obtained as input. Temperature dependencies of magnetic susceptibility of NiC synthesized have been studied up to 950 K. Carbides synthesized were found to be weak ferromagnets at the room temperature and their Curie temperature T_C ranges within 670 – 725 K. The calculated value of the magnetic moment per nickel atom (2.83μ_B) is higher than that of a bulk Ni (1.3μ_B). Likely, the observed increase of μ is caused by the presence of a certain amount of residual single-domain ferromagnetic Ni nanoparticles in the samples synthesized.     

新型纳米晶FexC系软磁合金粉末的制备及磁性研究

用机械球磨方法(MA)制备纳米晶FexC系软磁合金粉末(其中x=1、3、4、8),球磨时间分别为60、120、180、255、300h.用X-ray衍射谱分析样品的物相及其晶格结构,用振动样品磁强计测量粉末样品的磁性.对不同球磨时间而言,发现当球磨时间在小于120h范围内,随着球磨时间的增加,样品的软磁特能不断提高,当球磨时间达120h时,材料有最佳的软磁特能,对不同球磨成分而言,随着C含量减少(Fe含量的增加),其磁性能进一步提高,当x=8时,材料的饱和磁化强度σs达178.24emu/g,矫顽力降为1.76kA/m.其优良的软磁特性可与传统的FeNi、FeCo合金粉末相比.当球磨时间大于120h,样品的软磁性能开始变差.从X-ray衍射谱的分析可看出,这是由于样品发生了相变,从单相体心立方结构的α-Fe(C)固溶体向FeC金属间化合物转变.x=1的样品,经255h球磨后,样品成为单相Fe5C2金属间化物,它具有单斜晶体结构.这说明随着球磨时间的增加,材料由软磁性向硬磁性转化.同时发现样品随C含量增加时材料的抗氧化能力也提高了.并对上述实验结果进行了讨论.     

机械合金化-放电等离子烧结Al2Cu颗粒增强Al基复合材料的制备

以Al粉和Cu粉为原料,采用机械合金化(MA)和放电等离子烧结(SPS)工艺,原位合成了致密的Al₂Cu/Al块体复合材料,着重研究了MA过程中粉末的形貌、尺寸和物相结构的变化以及SPS后复合材料的微观组织和力学性能。结果表明: 在MA过程中,随着MA时间延长,部分Cu原子逐渐固溶于Al原子晶格中,形成均匀过饱和的固溶体Al(Cu);在SPS过程中,Cu从过饱和固溶体中析出并与Al反应形成Al₂Cu颗粒,且弥散分布于Al基体中,形成Al₂Cu/Al复合材料;Al₂Cu/Al复合材料的致密度高达98.7%,室温下的压缩断裂强度为611.3 MPa,延伸率为9.6%,具有良好的力学性能。     

Formation of B2 intermetallic NiAl and FeAl by mechanical alloying

Nanostructud B2 intermetallic compounds NiAl and FeAl have been prepared by mechanical alloying (MA) the elemental powder mixtures and subsequent heating. The structural evolution during MA was monitored by in situ thermal analysis and X-ray diffraction (XRD). The final products were characterized by transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The results show that the nanocrystalline intermetallic compound NiAl, which is difficult to disorder by milling, was synthesized directly after an exothermic explosive reaction; whereas FeAl compound was formed after a thermal process of asmilled Fe(Al) solid solution obtained through interdiffusion during MA. The large heat of formation of NiAl compound is the main driving force for the exothermic explosive reaction, and the difference in diffusivity between NiAl system and FeAl system is suggested to be the main cause of the different behaviors of formation between NiAl and FeAl compounds by MA.     

Microstructural characterization of medical-grade stainless steel powders prepared by mechanical alloying and subsequent annealing

The harmful effect of nickel ions released from conventional stainless steel implants has provided a high level of motivation for the further development of nickel-free stainless steels. In this paper, the microstructure of medical-grade nickel-free stainless steel powders, with the chemical composition of ASTM F2581, is studied during mechanical alloying and subsequent annealing. Rietveld X-ray diffraction and transmission electron microscopy evaluations reflect nanocrystallization, austenitization and amorphization of the powders due to mechanical activation. It is also realized that annealing of the as-milled powder can develop a single austenitic structure with nanometric crystallite sizes, implying a considerable inherent resistance to grain growth. This study demonstrates the merit of mechanical alloying and subsequent annealing in the development of nanostructured medical-grade stainless steels.     

Improvement of microstructure and mechanical properties of AZ91/SiC composite by mechanical alloying

AZ91 magnesium alloy reinforced with SiC particulates was fabricated via powder metallurgy technique as well as mechanical alloying process where a planetary ball mill was employed. Microstructure and mechanical properties of the fabricated AZ91 composites had been evaluated. Microstructural study showed that grain size of the material was refined and SiC particulates were well distributed after mechanical alloying. Mechanical tests of the composite showed an enhanced yield and ultimate tensile strengths for the mechanically alloyed samples compared with those prepared via the powder metallurgical route.     

W-Y2O3 composites obtained by mechanical alloying and sintering

The aim of this work was to manufacture tungsten composites from different initial powder mixtures by mechanical alloying followed by sintering. Two initial powder mixtures, W + 5 wt% of Y₂O₃ and W + 10 wt% of Y₂O₃, and pure W for comparison were mechanically alloyed for 50 h in a Fritsch Pulverisette P5 planetary ball mill under an argon atmosphere. The final products were consolidated by pulse plasma sintering at 1640 °C under a pressure of 20 MPa. The powders and consolidated pellets were examined by the XRD method. The obtained results show that during milling, the tungsten based solid solution formed. After consolidation, the XRD examination revealed that in addition to the tungsten-based solid solution and yttria, new carbide phases (Fe₃C, WC, W₂C and Fe₃W₃C) appeared. The graphite present in the carbides originated from the die used in the sintering process. SEM observations of the surfaces of the sinters revealed that the microstructure is not homogeneous and consists of areas rich in one or two elements, such as W, C, Fe or the Y₂O₃ phase. The microhardness of the pellets increases with the increasing content of the Y₂O₃ strengthening phase, whereas the values of the relative density decrease.     

机械合金化后注射成形制备Cu/Al2O3复合材料的显微组织与力学性能

采用机械合金化后注射成形制备10%(体积分数,下同)Cu/Al_2O_3复合材料,研究机械合金化时间、烧结温度对复合材料显微组织和性能的影响,并分析复合材料的增韧机理。结果表明:通过机械合金化10h后注射成形、脱脂、1550℃烧结工艺制备的10%Cu/Al_2O_3复合材料具有良好的抗弯强度和断裂韧度,分别为532MPa和4.97MPa·m^1/2;烧结温度低于1550℃导致原子在固态下扩散能力不足,烧结温度高于1550℃则使颗粒边界移动速率大于孔隙逸出速率,二者都造成复合材料孔隙率增加,而导致材料的强度和韧度下降;机械合金化时间延长使复合材料晶粒细化、Cu与Al_2O_3之间的结合强度提高,材料强度和硬度提高,但断裂韧度下降;Cu粉末弥散分布于Al_2O_3基体中,抑制烧结过程中Al_2O_3晶粒粗化,且使裂纹在扩展过程中遇到延性的Cu产生裂纹桥联和偏转,提高材料的韧度。     

Solid state amorphization of Mg-Zn-Ca system via mechanical alloying and characterization

Magnesium based bulk metallic glasses have attracted significant attention of researchers due to better mechanical and corrosion properties when compared to their crystalline counterparts especially for biomedical applications. Scaling up the part size and production volumes of such materials through liquid metallurgy route is challenging. In this work amorphous Ca₅Mg_60+xZn_35?x (X = 0, 3 and 7) alloys have been successfully synthesized through solid state amorphization using a high energy planetary ball mill. X-ray diffraction was used to identify the crystalline phases of the powder during reaction. Evolution of amorphous phase was analysed using a parameter involving the ratio of integral area of peaks to the integral area of background (I_PB) obtained from XRD patterns. Results showed reaction time increases with decreasing Zn content in Ca₅Mg_60+xZn_35?x (X = 0, 3 and 7) alloy to obtain maximum amorphous structure with a small amount of residual crystalline phase. Prolonged milling of these powders, to eliminate residual crystalline phases, resulted in the nucleation of Mg_102.08Zn_39.6 phase. The composition dependent characteristic temperatures and thermal stabilities were studied using differential scanning calorimetry.     

Phase transformations of NbCr2 intermetallics produced by mechanical alloying followed by hot-pressing consolidation

Mechanical alloying followed by hot-pressing consolidation has been used to produce NbCr₂ intermetallics under different conditions. High-purity Nb and Cr crystalline powders, in the relative (molar) ratio of 13:1, were milled for periods up to 100 h. This powder was vacuum-sintered at temperatures ranging from 1423 to 1573 K for 0.5 h under a pressure of 45 MPa. The phase transformations of the NbCr₂ were investigated by X-ray diffraction and scanning electron microscopy; several different phase transformations were observed. Increasing the milling time up to 100 h transforms into a mixture of C14, Nb, Cr and C15. The experimental results show that new evidence based on X-ray diffraction measurements further establishes the existence of a high-temperature C14 Laves polytype; an intermediate C36 structure for NbCr₂, reported in the literature, was not detected in this study. The relationship between the various phase transformations, based on the atomic radii and different preparation techniques, is discussed.     

Discharge properties of Mg2Ni-Ni alloy synthesized by mechanical alloying

The electrochemical characteristics of Mg₂Ni-Ni alloys prepared by mechanical alloying (MA) using a planetary ball mill were investigated. The discharge capacity depends on the molar ratio in Ni andMg₂Ni, and it has a maximum value of about 480 mAh/g at the equimolar ratio of Ni/Mg₂Ni. This discharge capacity (480 mAh/g) is about 74% of the theoretical one. The discharge capacity is reduced to about half within five cycles. Thus, the cycle time would be improved by inhibiting the oxidation of Mg₂Ni.     

New materials produced by mechanical alloying

The application of mechanical alloying (MA) to alloys based on Fe, Cu, Al, Ti, Co, Ni, Mg, and Nb is reviewed. Enhancement in physical and mechanical behavior, beyond ingot metallurgy and rapid solidification levels, can be achieved by MA, and should lead to commercialization of a number of MA alloys.Conducted under the joint Moscow-Moscow program on Synthesis of Advanced Materials (SAM).     

Positron annihilation characterization of Fe-Y2O3 composite powder after mechanical alloying and heat treatment

Fe-1 wt% Y2O3 composite powders were mechanically alloyed for 12 hr and then heat-treated at 1050 degrees C for 1 hr. Positron annihilation lifetime and coincidence Doppler broadening measurements are in qualitative agreement with X-ray diffraction studies, indicating that in the as-mixed Fe-1Y2O3 composite, up to approximately equal to 70% of the annihilations occur at vacancy clusters; a small fraction annihilates in its matrix. In the case of mechanically alloyed composite, up to approximately equal to 60% of the positrons annihilate at vacancy clusters. Some annihilations also occur in dislocations. In the heat-treated Fe-1Y2O3, positrons primarily annihilate at yttria precipitates, while a small fraction annihilates in the matrix.