On the Use of Ball Milling for the Production of Ceramic Powders

In the present research work, the mixture of boron carbide and graphite ceramic powders with a theoretical composition of 50% each by weight were mechanically alloyed in a laboratory ball mill with different milling times of 12.5, 25, 50, 75, and 100 h. The investigation was carried out on the morphologies and densities of ball-milled powders. Morphology results revealed that ball milling is a very dominant and dynamic practice for preparation of two different powders into single entity powder having appropriate and consistent morphology. The results of density measurement showed that with milling times, density increased initially and then reduced with further increase in milling times. The density is reduced by 1.68% as the milling time increased from 0 to 100 h.     

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.     

Comparative study on sintering behavior of Al86Ni6Y4.5Co2La1.5 mechanically alloyed amorphous powder and melt-spun ribbon

In this research work, the sintering characteristics of Al₈₆Ni₆Y_4.5Co₂La_1.5 mechanically alloyed amorphous powders and milled melt spun ribbon have been compared. Mechanically alloyed amorphous powders were synthesized via 200?h high energy ball milling. Melt spun ribbons were synthesized by single roller melt spinning technique and grounded to powder form by ball milling. Mechanically induced partial crystallization occurred in the ribbons during milling. Significantly higher amount of contaminations such as carbon, oxygen and iron were observed in the mechanically alloyed amorphous powders compared to the milled ribbons. Both powders were consolidated via spark plasma sintering. Superior particle bonding was found in the sample consolidated from milled ribbons, ascribed to the lower amount of contamination that could not effectively restrict the viscous flow and diffusion of atoms. Various complex crystalline phases evolved in the sample consolidated from milled ribbon particles due to the presence of crystalline phases in the powders which acted as nucleation sites, whereas the amorphous phase was mostly retained in its counterpart. Vickers microhardness of the consolidated alloys from milled ribbon and mechanically alloyed amorphous powders were 3.60?±?0.13?GPa and 2.53?±?0.09?GPa, respectively. The higher hardness in the former case was attributed to the superior particle bonding and distribution of hard intermetallic phases in the amorphous matrix.     

Ball milling of Co70 Fe8Si9B13 amorphous ribbon,crystallized ribbon and a mixture of pure crystalline powders

Co₇₀ Fe₈ Si₉B₁₃ amorphous ribbon, crystallized ribbon and a mixture of pure crystalline powders were mechanically alloyed by milling and nanocrystalline structures were obtained. The structural changes were monitored By X-ray diffraction and differential scanning calorimetry measurements. The thermal behaviour on heating the alloys prepared by ball milling was studied and the influence of the high-energy ball milling on the resulting phases was found.     

Powder Metallurgical Fabrication and Characterization of Nanostructured Porous NiTi Shape-Memory Alloy

Production of NiTi alloy from elemental powders was conducted by mechanical alloying (MA) and sintering of the raw materials. Effects of milling time and milling speed (RPM) on crystallite size, lattice strain, and XRD peak intensities were investigated by X-ray analysis of the alloy. Powder compaction and sintering time and temperature effects on pore percentage of the as-mixed and the mechanically alloyed samples were empirically evaluated. The crystallite size of the mechanically alloyed Ni₅₀Ti₅₀ samples decreased with MA duration and with the milling speed. Depending on the crystal structure of the raw materials, the lattice strain increases with the milling duration. Metallographic studies proved the existence of martensitic B19' after sintering of both the as-mixed and the mechanically alloyed samples. Its amount was, however, greater for the former. Sintering lowered the porosity of the samples; no matter what powder (as-mixed or mechanically alloyed) was used. The porosity was greater, however, for the MA powders. This difference seemed to be due to the sharper liquid phase sintering effect of the as-mixed samples.     

Accelerated mechanical alloying of mutually insoluble metals: Co-Cu system

We propose a new method for accelerating the process of mechanical alloying in the Co-Cu system possessing positive enthalpy of mixing and exhibiting no mutual solubility of components under equilibrium conditions. For this purpose, highly disperse powders of composite particles representing a Co-P amorphous alloy core covered with a nanocrystalline copper shell were prepared by chemical deposition. These composite powders were mechanically alloyed by processing in a ball mill. Investigation of the atomic structure and magnetic properties of the composite powders upon milling showed that the formation of supersaturated Co-Cu solid solutions under such conditions requires a much shorter milling time as compared to that for the conventional mechanical alloying processes.     

Synthesis and Characterization of Nanocrystalline Ni-Ti and Ni-Cr Powders by Mechanical Alloying

Nanocrystalline powders in the Ni-Ti and Ni-Cr systems were prepared by mechanical alloying (MA) of elemental crystalline powders in an inert atmosphere. The microstructure of the mechanically alloyed powders were characterized by XRD and TEM. The ball-milling process results in a drastic decrease of the crystallite size to the nanometer scale. X-ray diffraction analysis reveals that in the Ni-Cr system, no diffraction peaks from NiCr compound were observed even after 20 h of ball milling; while the lattice parameter of Ni increased with the milling time. In the Ni-Ti system, amorphous alloy was formed. Crystalline intermetallic compounds were obtained by post heat treatment of the amorphous alloy.The crystallization temperature of the amorphous NiTi alloy was obtained be DSC measurement.     

Electrocatalytic properties of mechanically alloyed Co-20wt%Ni-10wt%Mo and Co-70wt%Ni-10wt%Mo alloy powders

Mechanically alloyed Co-20wt%Ni-10wt%Mo and Co-70wt%Ni-10wt%Mo (nominal compositions) alloy powders were produced by milling of pure elemental powders. Mechanically alloyed powders were characterized by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. MA powder specimens were tested electrollitically in a 30% KOH aqueous solution at 298 K. X-ray diffraction analysis and transmission electron microscopy of milled powders showed the presence of two phases, an fcc solid solution and intermetallic compounds of Ni or Co with Mo. These phases showed a nanometric size. The linear sweep voltammograms confirmed also the presence of two phases in both mechanically alloyed alloy powders. The Co-20wt%Ni-10wt%Mo alloy powders showed the best electrocatalytic activity for hydrogen evolution reaction.     

Formation of Magnesium Silicide by Mechanical Alloying

Elemental Mg and Si powders were mechanically alloyed in a planetary ball mill. The formation of magnesium silicide as well as the formation of magnesium oxide and hydride in the milled powders was studied in detail by X-ray diffraction and scanning differential calorimetry. It was found that direct formation of the magnesium silicide, Mg₂Si, occurred after 10 hours of milling and the content of Mg₂Si increased with increasing the milling duration. The activation energy for the formation of Mg₂Si was calculated by the Kissinger approach to be 215 kJ/mol. Besides oxidizing and hydrizing of Mg by decomposed organic additives during mechanical alloying, an increased contamination of powders from steel and alumina milling tools with increasing milling duration was detected. A short milling duration followed by a thermal treatment was thus suggested to synthesize magnesium silicide.     

高能球磨时间和退火温度对制备TiNi合金粉的影响

为获得高能球磨时间和退火温度对TiNi机械合金粉特性的影响机制,采用X射线衍射(XRD)、扫描电子显微镜(SEM)、X射线能谱仪(EDS)、差示扫描量热法(DSC)等分析方法对TiNi合金粉进行了研究。结果表明,机械合金的相成分随着在氩气保护气氛中的球磨时间和退火温度的不同而发生变化。球磨22h的产物是非晶态TiNi合金、Ti的固溶体、Ni的固溶体,球磨27h的产物是非晶态TiNi合金粉和Ni固溶体相,球磨30h发生了明显的固相反应,生成了TiNi、Ni3Ti、Ti3Ni4等物相;在650℃/5h和1000℃/5h下的退火产物都是Ni3Ti、Ti2Ni、TiNi2、TiNi和TiC,但在上述2个退火温度下TiNi并不是主要物相,其中在650℃退火时TiNi的含量明显更低。     

Mechanically alloyed Ni/8YSZ powder mixtures: preparation, powder characterization and sintering behavior

A state of the art anode for the solid oxide fuel cell (SOFC)consists of a mixture of 8 mol % Y2O3-stabilized zirconia (8YSZ) andnickel particles, which form an interconnected porous structure after sintering. Coarsening of the Ni particles under SOFC workingconditions has to be avoided, hence it leads to a deterioration of the anode's performance. In the present work the aim was to improve thestability of the Ni particles by a reduction of the sinteringactivity of nickel. For this purpose between 10 and 50 % by volume of nano-sized zirconia particleshave been dispersed in the nickel matrix by dry ball milling in a planetary mill.Forpressed samples made of mechanically alloyed Ni with 10 vol % of 8YSZ,a homogeneous dispersion of 8YSZ particles in the Ni matrix wasconfirmed by transmission electron microscopy. It was confirmed bymercury porosity penetration and optical microscopy that thisdispersoid structure leads to a retardation of recrystallization.Also, an essentially lowered densification during sintering was found, compared to samples made of the pure Ni powder. Samples made of mechanically alloyed Ni with a higher zirconia amountshowed a higher densification during sintering and annealing thansamples containing 10 vol % 8YSZ. It is assumed that this results frominsufficient dispersion in these systems. The results show that mechanically alloyed nickel,with a homogeneous dispersion of 8YSZ crystallites, is a promising candidate for high temperature catalysts.     

Sintering behavior of mechanically alloyed Ti-48Al-2Nb aluminides

Ti-Al intermetallics have been produced using mechanical alloying technique. A composition of Ti-48Al-2Nb at % powders was mechanically alloyed for various durations of 20, 40, 60, 80 and 100 h. At the early stages of milling, a Ti (Al) solid solution is formed, on further milling the formation of amorphous phase occurs. Traces of TiAl and Ti₃Al were formed with major Ti and Al phases after milling at 40 h and beyond. When further milled, phases of intermetallic compounds like TiAl and Ti₃Al were formed after 80 hours of milling and they also found in 100 h milled powders. The powders milled for different durations were sintered at 785°C in vacuum. The mechanically alloyed powders as well as the sintered compacts were characterized by XRD, FESEM and DTA to determine the phases, crystallite size, microstructures and the influence of sintering over mechanical alloying.     

不同晶粒尺寸的三元Cu40Ni40Cr20合金的制备及其显微组织研究

采用电弧熔炼和机械合金化,随后在750℃,58MPa下热压制备了晶粒尺寸差别较大的Cu40Ni40Cr20合金,用X射线衍射仪、扫描电镜等分析手段对比研究了显微组织结构.结果表明:电弧熔炼制备的晶粒尺寸较大的Cu40Ni40Cr20合金为二相,组织极其不均匀;采用机械合金化,通过控制热压条件制备的纳米晶Cu40Ni40Cr20合金仍为双相,但显微组织均匀,稳定.随着球磨时间的延长,由于晶粒细化和应变的结果,衍射峰偏移并有明显的宽化产生,Cu在Cr或Cr在Cu中的固溶度明显增加,当球磨60h后,合金已由双相变成亚稳态的单相.由于机械合金化的粉末处于非平衡态,其超固溶度溶质随热压和真空退火过程的进行会慢慢脱溶分解出来,合金已由单相变为两相,两相颗粒均成倍长大,但仍然保持纳米级尺度;机械合金化、热压和退火后样品中Cu,Ni和Cr的晶格均未发生崎变;讨论了晶粒细化对合金显微组织的影响.     

Effect of ball milling time on the structural characteristics and mechanical properties of nano-sized Y2O3 particle reinforced aluminum matrix composites produced by powder metallurgy route

Mechanical milling presents an effective solution in producing a homogenous structure for composites. The present study focused on the production of 0.5 wt% yttria nanoparticle reinforced 7075 aluminum alloy composite in order to examine the effects of yttria dispersion and interfacial bonding by ball milling technique. The 7075 aluminum alloy powders and yttria were mechanically alloyed with different milling times. The milled composites powders were then consolidated with the help of hot pressing. Hardness, density, and tensile tests were carried out for characterizing the mechanical properties of the composite. The milled powder and the microstructural evolution of the composites were analyzed utilizing scanning and transmission electron microscopy. A striking enhancement of 164% and 90% in hardness and ultimate tensile strength, respectively, were found compared with the reference 7075 aluminum alloy fabricated with the same producing history. The origins of the observed increase in hardness and strength were discussed within the strengthening mechanisms' framework.     

Changes in the oxygen content,morphology, and microstructure of Mo-10Nb composite powders during mechanical alloying

The prefabrication of Mo-Nb composite powders is an effective way of improving the homogeneity of Mo-10Nb targets, which have broad application prospects in the photoelectric sensor industry. However, this aspect has been rarely addressed so far. Therefore, we prepared Mo-10Nb composite powders by mechanical alloying (MA), and investigated the effects of the experimental parameters such as the milling speed and duration on the particle morphology, size distribution, compositional homogeneity, crystallite size, inner strain, and oxygen content. High-quality Mo-10Nb composite powders with 3-μm spherical particles of narrow size distribution, homogeneous elemental distribution, and nanometric crystalline structure were obtained by implementing optimum MA parameters, viz., a milling speed of 250 rpm and duration of 36 h using an MITR QM-QX-4L omnidirectional ball mill. The mechanically alloyed Mo-10Nb composite powders were prone to oxidation when exposed to air, which led to a sharp increase in the oxygen content to ~5400 ppm. X-ray photoelectron spectroscopic analysis revealed the presence of Nb₂O₅, MoO₂, and MoO₃ on the surface of the Mo-10Nb particle. We believe that this study demonstrates an interesting strategy for the fabrication of high-quality Mo-10Nb targets.     

Structure and Magnetic Properties of Powders Prepared by Mechanically Alloying 50Fe + 25Al + 25Si Mixtures

A 50Fe + 25Al + 25Si powder mixture was mechanically alloyed in a high-energy ball mill, and the products of the solid-state reactions were characterized by x-ray diffraction and magnetic measurements. The results show that the process involves the formation of a metastable bcc FeAl,Si solid solution, which decomposes into the ordered phases FeAl_{1 – x} Si _x (B2 structure) and FeSi (B20) upon heating to 700°C or long-term milling. The observed effect of milling on the magnetic properties of the powders indicates that the proportion of the ferromagnetic component in the alloy decreases with increasing milling time as a result of the ordering of the solid solution and the formation of the B2 and B20 paramagnetic phases.     

Formation of a FCC Al_(54)Ti_(23)C_(23) Metastable Phase by Ball Milling

The powder mixture of Al, Ti and graphite has been mechanically alloyed in a planetary ball mill.The structural evolution of as-milled powder sample has been characterized by XRD, DTA. The results show that the amorphous phase is formed first at an early milling stage, then crystallization occurs during further milling, leading to formation of a nanocrystalline fcc metastable phase. In contrast, during annealing the amorphous phase is crystallized to the equilibrium phase instead of the fcc phase. This indicates that crystallization during ball milling is different from that induced by annealing     

Sintering of nanostructured W-Cu alloys prepared by mechanical alloying

Nanostructured (NS) powders with compositions corresponding to W-20wt%Cu and W-30wt%Cu were prepared by mechanical alloying. The microstructure and grain size of as-milled and annealed powders were analyzed by transmission electron microscopy. The compacted specimens were sintered at temperatures in the range 1000 °–1300 °, and then the microstructures of sintered parts were analyzed by scanning electron microscopy. Sintering of mechanically alloyed W-Cu alloys appears to be independent of Cu content, and may be explained in terms of recovery and grain growth in the mechanically alloyed powders as well as impurity activated sintering of W. After sintering, Cu pools are formed outside the mechanically alloyed powders. A relative sintered density of more than 95% is obtained by particle rearrangement during liquid-phase sintering, and the greatest homogeneity of W and Cu phases is achieved by sintering at 1200 °.     

Synthesis of Ti-based bulk quasicrystal by shock compression

We attempted to produce a Ti₄₅Zr₃₈Ni₁₇ bulk icosahedral (i) quasicrystal by a shock compression technique, in which a single-stage powder gun discharges a flyer plate that consolidates the target powders. The results were also compared with those by a conventional hot-pressing. The powder mixtures for the shock compression were blended by two kinds of methods; that is, gently mixing in a vial, and mechanically alloying by a planetary ball mill. A large bulk i-phase sample, with a Ti₂Ni crystal phase, was synthesized from mechanically alloyed powders after shock compression at a higher flyer velocity, although the conventional hot-pressing at 3 MPa synthesized only the Ti₂Ni phase. For the gently mixed powders, no reaction occured even after shock compression. High-pressure and high-temperature produced during shock compression, and milling process were key factors to obtain the i-phase. The Vickers hardness and the wetting contact angle with pure water under an atmospheric pressure for the bulk sample containing the i-phase were about 7 GPa and about 70°, respectively.     

The reaction of hydrogen with Mg-Cd alloys prepared by mechanical alloying

In this paper, we present the hydrogen storage properties of Mg-Cd alloys prepared by ball milling. Mechanical alloying of a mixture of Mg and Cd elemental powders containing up to 20 at.%Cd leads to a magnesium solid solution. The lattice spacings of the hcp Mg phase shrink with dissolution of cadmium atoms in Mg. The mechanically alloyed pure Mg-Cd alloys are very difficult to activate for hydrogen absorption. However, if vanadium and graphite additives are added, a Mg(Cd)-V-C nanocomposite forms after ball milling and the activation then becomes very easy. The hydrogen absorption/desorption kinetics are very fast. The plateau pressure and slope of hydrogen absorption/desorption increase, while the hydrogen storage capacity decreases with increasing cadmium content.