Synthesis of BF–PT perovskite powders by high-energy ball milling

0.7BiFeO₃–0.3PbTiO₃ (BF–PT) powders were synthesized from a mixture of the oxides Bi₂O₃, Fe₂O₃, PbO and TiO₂ using a Fritsch P4™ vario-planetary ball milling system. The perovskite structure of the BF–PT powder can be obtained well and the crystallite size of the powders was greatly reduced to 20–35 nm after milling for 8 h. The pre-calcined course shows a rhombohedral–tetragonal phase transition with the increasing temperature and shows the structure transition near the Curie temperature T_c.     

Microstructural characterization of amorphous and nanocrystalline boron nitride prepared by high-energy ball milling

Microstructural parameters like crystallite size, lattice strain, stacking faults and dislocation density were evaluated from the X-ray diffraction data of boron nitride (BN) powder milled in a high-energy vibrational ball mill for different length of time (2-120 h), using different model based approaches like Scherrer analysis, integral breadth method, Williamson-Hall technique and modified Rietveld technique. From diffraction line-broadening analysis of the successive patterns of BN with varying milling time, it was observed that overall line broadening was an operative cause for crystallite size reduction at lower milling time (∼5 h), whereas lattice strains were the prominent cause of line broadening at higher milling times (>19 h). For intermediate milling time (7-19 h), both crystallite size and lattice strain influence the profile broadening although their relative contribution vary with milling time. Microstructural information showed that after long time milling (>19 h) BN becomes mixture of nanocrystalline and amorphous BN. The accumulations of defects cause this crystalline to amorphous transition. It has been found that twin fault (β′) and deformation fault (α) significantly contributed to BN powder as synthesized by a high-energy ball-milling technique. Present study consider only three ball-milled (0, 2 and 3 h) BN powder for faults calculation because fault effected reflections (1 0 1, 1 0 2, 1 0 3) disappear with milling time (>3 h). The morphology and particle size of the BN powders before and after ball milling were also observed in a field emission scanning electron microscope (FESEM).     

高能球磨法制备超滤分离膜用钼铜复合粉末

研究高能球磨法制备纳米钼铜复合粉末的主要影响因素,通过扫描电镜和透射电镜分析粉末的形貌及颗粒尺寸.研究结果表明,复合粉的粒度随着球磨时间的延长而减小,但随着球磨时间增加,团聚加剧;通过重力沉降法可以去除浆体中的团聚体,从而获得颗粒分布适合的粉体,10h球磨粉沉降后粉体颗粒尺寸约为50～60nm,20h球磨粉沉降后粉体颗粒尺寸约为20～30nm.     

Incontinuous grain growth in cobalt nanocrystalline powders prepared by high-energy mechanical milling

Cobalt nanocrystalline powders with the average grain size of about 17 nm were prepared by high-energy mechanical milling. Grain growth in highly pure and particle-containing nanocrystalline Co powders were investigated respectively by a series of annealing experiments at different temperatures. The characteristics of incontinuous grain growth were found in both the pure and the particle-containing nanocrystalline powders. It is proposed by the authors that the sharp increase in nanograin size in the transition between the low and high temperature regions is a result of enhanced grain growth promoted by the stored energy as a supplied driving force, based on which rapid grain growth occurs through a particular dominant mechanism of nanograin rotations in the pure nanocrystalline powders, and that through off-pinning of grain boundaries in the particle-containing nanocrystalline powders.     

Sub-micron sized Al2TiO5 powders prepared by high-energy ball milling

High energy ball milling to obtain ultrafine aluminium titanate particles has been investigated. Tempered steel has been selected as material for the containers and balls because the desirable properties of aluminium titanate are not degraded by small amounts of Fe₂O₃. The starting powders have been milled during different periods (1–60 h) and the evolution of the morphology and crystallinity of the treated powders as well as the extent of contamination from the milling media have been characterised. Different experimental techniques, X-ray diffraction, BET-analysis, chemical analysis, scanning electron microscopy and low and high resolution transmission electron microscopy have been used. High energy ball milling has been proved to be an efficient route to obtain submicron sized (50–100 nm) aluminium titanate powders, but further milling of the powders is accompanied by contamination from the milling media and the formation of hard agglomerates.     

Translucent PMN and PMN-PT ceramics from high-energy ball milling derived powders

Translucent PMN and PMN-PT ceramics were prepared from nano-sized powders produced by a high-energy ball milling process. A two-step process was used to achieve the translucent PMN and PMN-PT ceramics, in which samples were sintered at 950°C for 1 h at first and then annealed at 1100°C for 6-24 h. Transmittances at 600 nm wavelength of the PMN, PMN-0.10PT and PMN-0.35PT ceramics annealed for 12 h were 21, 16 and 11%, respectively. The formation mechanism of translucent PMN and PMN-PT ceramics in the present work is similar to that of transparent PLZT ceramics.     

Effect of ball milling parameters on the particle size in nanocrystalline powders

A model describing the mechanical comminution (ball milling) of crystals to nanocrystalline powders is proposed. It is shown that a fraction of the energy deposited in the processed material is spent for the creation of microstresses ?, which slows down the comminution process.     

Synthesis of Cu-W nanocomposite by high-energy ball milling

The Cu-W bulk nanocomposites of different compositions were successfully synthesized by high-energy ball milling of elemental powders. The nanocrystalline nature of the Cu-W composite powder is confirmed by X-ray diffraction analysis, transmission electron microscopy, and atomic force microscopy. The Cu-W nanocomposite powder could be sintered at 300-400 degrees C below the sintering temperature of the un-milled Cu-W powders. The Cu-W nanocomposites showed superior densification and hardness than that of un-milled Cu-W composites. The nanocomposites also have three times higher hardness to resistivity ratio in comparison to Oxygen free high conductivity copper.     

高能球磨固态扩散反应研究

从扩散理论出发,结合结合Ａｌ－Ｃｕ合金高能球磨实验结果,分析了高能球磨过程中的扩散特点,提出了固态合成反应模型并进行了分析计算,结果表明,高能球磨过程中固态反应能否发生取决于体系在球磨过程中能量升高程度,而反应完成与否则受体系中的扩散过程控制,即受制于晶粒细化攻粉末碰撞温度。     

机械球磨和烧结制备CoSb3的工艺研究

针对skutterudite材料制备工艺中熔融法和固相反应法合成周期长、工序多的不足,尝试将机械合金化法应用于skutterudite材料制备中.探讨了CoSb3的机械合金化和烧结制备工艺,研究表明,Co、Sb粉末的机械合金化在球磨10 h后开始,球磨40h后已全部合金化,得到CoSb,和CoSb2相混合物.合金化过程中CoSb3相先于CoSb2相形成.采用球磨10 h-700℃烧结2 h的工艺可得到单相CoSb3,制备工序简单,所需时间大大缩短.     

Nanostructure cathode materials prepared by high-energy ball milling method

We prepare Li₂MnO₃ and LiNi_0.5Mn_0.3Co_0.2O₂ as nanostructure cathode materials using a high-energy ball milling method with bulk-type electrodes. The nanostructure electrodes prepared by the ball milling exhibit much smaller particle sizes in diameter than those of bulk-type electrodes. The 1st charge–discharge capacitance and efficiency of the nanostructure cathode materials are superior to those of the bulk-type electrodes.     

Fast diffusion in nanocrystalline ceramics prepared by ball milling

Nanocrystalline materials can show enhanced diffusivity compared to their microcrystalline counterparts due to the large fraction of atoms or ions located in interfacial regions. In the case of ceramics, resulting properties with potential applications are, e.g., fast ionic conductivity, high mechanical creep rate and increased catalytic activity. Different nanocrystalline ceramic materials were prepared by high-energy ball milling of coarse grained source materials. The samples were characterized by XRD, TEM, BET method and IR spectroscopy. These measurements show that the primary crystallites form larger agglomerates with internal interfaces and that the reduction of the crystallite size is accompanied by a structural degradation of the surface zone. An example is the partial amorphization observed for LiBO₂ by IR spectroscopy. The diffusivity and ion conductivity in these materials was studied by NMR relaxation, NMR line shape and impedance spectroscopies. It was possible to discriminate between highly mobile ions in the interfacial regions and immobile ions in the grains. In general diffusion in the nanocrystalline systems was found to be fast compared to that in the corresponding microcrystalline source materials.     

Solid-state transformation in nanocrystalline Ti induced by ball milling

In the current study, we report for the first time a new Ti rhombohedral (trigonal) structure induced by HEBM and subsequent sintering. During ball milling of Ti powder, solid-state transformation does not only depend on the grain refinement but also on the successful deformation of the nano-sized crystallites due to high energy ball impacts. Thermal stability of Ti-nanocrystalline in FCC allotrope was investigated. Upon sintering, the unstable FCC restored back to the rhombohedral phase rather than to HCP. The appearance of HCP Ti after sintering could suggest that prolonged milling leads to dispersion of hard particles (HCP) into more ductile particles belonging to allotropic phases, and hence possibility of resurfacing on sintering.     

Reactive ball milling to produce nanocrystalline ZnO

Ball milling of zinc powders in oxygen atmosphere leads to nanocrystalline ZnO. The average grain size has a value of 9 nm. The zinc oxidation proceeds gradually. It is compared with the combustion oxidation reactions of metals (Zr, Ti, Fe and Sn) reported previously. We propose a new parameter ΔH/C_p(metal) instead of simplified adiabatic temperature to judge if the mechanochemical oxidation of a particular metal happens via gradual or combustion reaction.     

氧化铝高能球磨时机械力化学效应研究

研究了氧化铝在高能球磨过程中机械力化学效应的变化.机械力化学效应因子随球磨时间的变化可分为三个阶段:第一阶段主要是晶粒尺寸减小和显微应变增加同时进行;第二阶段主要是有效温度系数的增加;第三阶段主要是点阵膨胀至饱和.用溶解法比较了球磨前后氧化铝的活性,发现经球磨后,氧化铝在盐酸中的溶解活化能由18 kJ/mol降至4 kJ/mol,表面活化层增厚.     

高能球磨锐钛矿型TiO2晶型转变的研究

应用机械力化学原理，研究高能行星磨粉磨锐钛矿型TiO2引起晶型转变的过程，采用XRD、SEM、TEM、FT－IR技术对粉体进行表征，探讨了机械力化学引起晶型转变的机制。研究发现：在一定操作参数（行星磨公转转速300r/min)条件下，粉磨初期（5h)为无定形形成期，颗粒出现团聚现象，晶粒尺寸减小，晶格畸变，转变为无定形，并形成金红石型TiO2晶核；粉磨中期（5－15h)为晶粒长大期，金红石型TiO2晶粒长大；粉磨后期（15h以后）为动态平衡期，晶粒长大与粉磨引起的晶粒减小处于动态平衡，研究表明；行星磨粉磨锐钛矿型TiO2可使晶型转变为金红石型TiO2，团聚的二次颗粒尺寸为1μm左右，并由颗粒尺寸为20－40nm团聚组成。     

Structural evolution of B2-NiAl synthesized by high-energy ball milling

Structural evolution during the synthesis of B2–NiAl intermetallic compound by mechanical alloying of equiatomic elemental mixtures was studied by Rietveld analysis, DSC and HTXRD. The lattice parameter, crystallite size, microstrain, amount of phase and ordering of the B2 phase were monitored as a function of milling time. Formation of the B2–NiAl phase shows a sigmoidal behavior, which suggests that Johnson–Mehl–Avrami nucleation and interface-controlled growth are the responsible mechanisms in the transformation. Almost complete transformation (~ 97 mol%) was obtained after 25 h of milling. A specific phase transformation sequence during milling was not absolutely determined, however, the sequence Ni + Al → NiAl₃ → Ni₂Al₃ → B2–NiAl was identified by HTXRD. This sequence was confirmed by DSC. The transformation temperature of the B2–NiAl phase and the presence of additional intermetallic compounds show a direct dependence on the Ni–Al layer spacing. Using a production-scale Simoloyer horizontal Attritor Mill, the presence of Ni₂Al₃ phase was observed prior to the full synthesis of B2-NiAl.     

高能球磨Ti/Al复合粉体低温烧结膨胀开裂行为

为了制备高密度的TiA l基合金,研究了高能球磨Ti/A l复合粉体的烧结性能.冷压坯在660℃以下真空反应烧结,采用排水法测定了烧结坯体积和密度变化,利用X射线衍射、扫描电子显微镜研究了坯料烧结过程中的相变和显微组织特征.结果表明,坯料在低温烧结过程中产生明显的体积膨胀和开裂.原因主要是低密度过渡金属间化合物TiA l3的形成,烧结过程中A l向Ti扩散留下的孔隙,高能球磨和压坯过程中产生的塑性变形以及Ti、A l反应烧结过程中的自蔓燃现象.适当延长球磨时间和严格控制烧结温度将有助于减少膨胀,避免开裂.