球磨时间对MA-SPS法制备FeCoCrAlNiB高熵合金微观结构、硬度和断裂韧性的影响

采用机械合金化(MA)和放电等离子烧结(SPS)相结合的方法制备FeCoCrAlNiB高熵合金。研究球磨时间(1、5、10、20、30和40 h)对合金相成分、微观结构、硬度和断裂韧性的影响。结果表明：高能球磨过程中各金属元素的合金化顺序为Al→Co→Ni→Fe→Cr;混合粉末球磨20 h后基本形成了单一的BCC固溶体相,其颗粒尺寸约为20μm。对不同球磨时间的混合粉末进行SPS烧结,获得的FeCoCrAlNiB高熵合金主要由无序BCC+B2(Al-Ni)固溶体相和硼化物相(Fe₂B等)组成。随着球磨时间的延长,合金中硼化物相含量先减少后增加并主要以网状形式分布,BCC相含量则与之相反;合金硬度随球磨时间的延长逐渐提高,主要是因为合金元素间固溶程度越来越高,硼化物相逐渐增多;但硼化物形成的网状结构会破坏基体的连续性,导致合金断裂韧性逐渐降低。当球磨时间为20 h时,获得的FeCoCrAlNiB高熵合金的维氏硬度(HV)为(10.9±0.2) GPa,断裂韧性(K_IC)为(4.4±0.2) MPa·m^1/2,表现出最优的综...     

高能球磨Mg-Zr-Ni合金组织演变

为了改善Mg-Ni合金的电化学性能,采用高能球磨技术合成了Mg-Zr-Ni储氢合金,通过改变球磨条件和添加合金元素Zr,利用XRD物相分析和电化学测量技术,研究了Mg-Ni合金的组织演变过程及其对电化学容量的影响.结果表明,高能球磨Mg-Ni和Mg-Zr-Ni合金都经历了非晶态向纳米晶态的转变过程,用少量Zr替代部分Mg后,促进了高能球磨Mg-Zr-Ni合金的非晶化和纳米晶化的过程.与非晶态Mg(Zr)Ni相比,纳米晶的Mg(Zr)Ni中氢更易放出,放电曲线主要呈现高电位放电特征,添加Zr后合金的放电容量有所下降.     

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。     

Improved critical current density in ex situ processed MgB2 tapes by the size reduction of grains and crystallites by high-energy ball milling

We have fabricated Fe-sheathed MgB₂ tapes through an ex situ process in a powder-in-tube (PIT) technique using powders ball milled under various conditions. Although the ex situ processed wires and tapes using the high-energy ball milled MgB₂ powders have been studied and the decrease of grain and crystallite sizes of MgB₂ and the critical current density (J_c) improvement of those conductors were reported so far, the use of filling powders milled at a higher rotation speed than previously reported further decreases the crystallite size and improves the J_c properties. The improved J_c values at 4.2 K and 10 T were nearly twice as large as those previously reported. Those milled powders and hence as-rolled tapes easily receive contamination in air. Thus, the transport J_c properties are easily deteriorated and scattered unless the samples are handled with care. The optimized heat treatment temperature (T_opt) of those tape samples at which best performance in the J_c property is obtained decreases by more than 100 °C, compared with that of tapes using the as-received MgB₂ powder.     

包覆混料对镀铜混合尺寸SiCp/Fe力学性能的影响

为探索提高SiCp/Fe力学性能的途径,采用包覆混料工艺,研究了该工艺对镀铜SiCp/Fe力学性能的影响,以及该工艺下增强粒子混合尺寸的影响.结果表明:包覆混料相比于普通混料,可显著改善SiC粒子在基体中分散的均匀性,而镀铜的作用是显著消除界面缺陷;性能的改善是包覆混料改善粒子分散性和镀铜改善界面结合的综合结果.对于体积分数30%SiCp/Fe的抗拉强度,通过包覆改善均匀性的贡献可提高7.2%,通过镀铜消除界面缺陷的贡献可提高12.5%,因此减少界面缺陷对颗粒增强复合材料力学性能的提高更重要.混合尺寸粒子对力学性能的增强效果明显高于其对应单一尺寸,这是由于小尺寸粒子能有效地提高基体的强度,而大尺寸颗粒更有效地承担载荷传递的作用.     

组元配比对球磨固态燃烧式反应和扩散型反应的影响

采用搅拌式高能球磨机研究了不同铝含量的Al/CuO球磨固态燃烧反应和Al-Cu及Al-Cu-Al2O3扩散型反应。结果表明：理想配比的Al/CuO的反应孕育期最短,偏离这一配比,孕育期延长,反应由整体燃烧式逐渐过渡到渐进燃烧式完成;球磨强度扩大以燃烧式进行的组元配比范围;当铝含量超过理想配比中的比例,随Al含量增加,反应由单一的还原反应向还原＋合成复合反应模式转化,反应产物为平衡组织,依次为Cu Al2O3、CuoAl4 Al2O3、CuAl2 Al2O3、Al(Cu) Al2O3;而球磨Al-Cu和Al-Cu-Al2O3体系的反应以扩散方式进行,产物是非平衡组织。     

Artificial neural network analysis of the effect of matrix size and milling time on the properties of flake Al-Cu-Mg alloy particles synthesized by ball milling

In this study, the effect of matrix size and milling time on the particle size, apparent density, and specific surface area of flake Al-Cu-Mg alloy powders was investigated both by experimental and artificial neural networks model. Four different matrix sizes (28, 60, 100, and 160?µm) and five different milling times (0.5, 1, 1.5, 2, and 2.5?h) were used in the fabrication of the flake Al-Cu-Mg alloy powders. A feed forward back propagation artificial neural network (ANN) system was used to predict the properties of flake Al-Cu-Mg alloy powders. For training process, the ANN models of the flake size, apparent density, and specific surface area have the mean square error of 0.66, 0.004, and 0.01%. For testing process, it was obtained that the R² values were 0.9984, 0.9998, and 0.9932 for the flake size, apparent density, and specific surface area, respectively. The degrees of accuracy of the prediction models were 95.145, 99.705, and 94.25% for the flake size, apparent density, and specific surface area, respectively.     

用高能球磨法制备的细晶Al-50Si合金的组织与性能

用高能球磨工艺制备Al-50Si合金粉末,将粉末经冷压、烧结、热压等工艺制备出Al-50Si合金块体材料,对球磨粉末和块体样品进行了显微组织观察、EDS分析和XRD分析,测定了块体样品的密度、硬度和热扩散系数.结果表明:高能球磨后Al-50Si合金粉末的硅粒子明显细化,其尺寸分布为1-15μm;在烧结过程中块体样品的硅粒子长大,其尺寸增大到5-30μm;Al-50Si合金块体材料具有较高的密度和硬度,其室温热扩散系数为55mm2·s-1.     

Effect of particle morphology on the flowability of HDH Ti powders treated by high temperature ball milling

The metal powder flowability determined by powder characteristics significantly influences on the final parts manufactured by additive manufacturing (AM). Among the characteristics, the individually effect of morphology on its flowability still is not comprehensively evaluated. In this study, the effect of morphology on the flowability of hydride-dehydrate titanium (HDH Ti) powder treated by high temperature ball milling (HTBM) was investigated systematically using the fractal dimension and shape factors, i.e., circularity, elongation, compactness and convexity. The results of HTBM show that the modified HDH Ti powder with a mass flow rate of 48.1 ± 0.3 s/50 g and the angle of repose (AOR) of 38.88 ± 0.5°. The fractal dimension of powder plays a main role on the flowability, which increase in the decrease of it. The box plot and Pearson correlation coefficient of shape factors indicate that only circularity is strong correlation with flowability, which increases with it. The regression model of flowability expressed with fractal dimension and circularity shows the adjusted R² value of 0.991, which is good agreement with the experiment. Taken together, this study provides a general guide to evaluate the powder flowability based on the morphology.     

Effect of ball size on milling efficiency of zinc oxide dispersions

Zinc oxide (ZnO) was wet milled using inert Al₂O₃-ceramic balls having different diameter at different milling intervals and the milling efficiency of the resultant dispersion was followed through particle size analysis and zeta potential measurements. The results indicated that small-sized balls improved the milling efficiency. The highest share (%) of lower-size particles was obtained after 24?h of ball milling.     

Effect of filler load and high-energy ball milling process on properties of plasticized wheat gluten/olive pomace biocomposite

The increase of particles surface area can optimize the dispersion state of biocomposite components and enhance their properties. First in this paper, we aimed to elaborate a novel biocomposite without any treatments. Plasticized wheat gluten (WG), was filled with 0–20% of olive pomace (OP) powder. The second objective was the improvement of biocomposite properties using physical treatment. High-energy ball milling process was applied on the blend of wheat gluten and olive pomace powders (MPs). The grinding effect of particle shape, size and distribution in biocomposite was characterised by particle size distribution using a laser-light diffraction and by SEM analysis. The cryo-fractured surface of selected films, mechanical properties, moisture absorption and thermal properties of both biocomposites were described in details. It was found that the sensitivity of biocomposites to moisture absorption was reduced with the increase of filler content after the applying of high-energy ball milling process. The thermal stability of OP biocomposite decreased with the increase of loading, while that of MPs was unaffected by high-energy ball milling process. This process affects the physical and morphological characteristics of the powders. The mechanical properties were improved by grinding process at filler content lower than15%.     

球磨时间对镁碳复合储氢材料结构和性能的影响

采用氢气气氛中高能球磨反应法,制备了40Mg60C镁碳复合储氢材料,研究了球磨时间对材料粒度、晶体结构和放氢性能的影响.结果表明,球磨2h材料的粒度即可达纳米级,约10～20nm,球磨时间再延长,材料团聚程度加重;球磨2h的材料为纳米晶和非晶结构,当球磨时间增加到4h时,材料几乎成为非晶结构;球磨时间4h时,材料储氢量已趋于饱和,最大放氢量为3.15%(质量分数);材料放氢温度随球磨时间的增加而降低,球磨5h材料的初始放氢温度和放氢峰温降为275.18和314.94℃.     

Microstructure evolution and interface structure of Al-40 wt% Si composites produced by high-energy ball milling

High silicon content Al-Si composites with a composition of Al-40 wt% Si were fabricated via a highenergy ball milling method. The microstructure evolution of Al-40 wt% Si milled powders and sintered composites has been thoroughly studied by scanning electron microscopy, X-ray diffraction, energydispersive spectrometry and high-resolution transmission electron microscopy. The mechanism of ball milling Al-40 wt% Si powders has been disclosed in detail: fracture mechanism dominating in the early stages, followed by the agglomeration mechanism, finally reaching the balance between the fragments and the agglomerates. It has been found that the average particle sizes of mixed Al-Si powders can be refined to the nanoscale, and the crystallite sizes of Al and Si have been reduced to 10nm and 62nm upon milling for 2h–50h, respectively. The finally formed Al-Si interfaces after ball milling for 50h are wellcohesive. A dense and homogenous Al-40 wt% Si composite have been achieved by solid-state sintering at550?C. The results thus provide an effective support for producing bulk nanostructured Al-Si composites.     

High purity synthesis of ZrB2 by a combined ball milling and carbothermal method: Structural and magnetic properties

The present work provides a new insight into the high purity synthesis of zirconium diboride (ZrB₂) powders and a method of controlling impurity during the synthesis process. The single phase ZrB₂ nano-powder was synthesized by a combined ball milling and carbothermal method using zirconium oxide (ZrO₂), boron oxide (B₂O₃) and carbon (C) as starting materials. The reaction pathway, phase purity, and morphology of the ZrB₂ produced are elucidated from X-ray diffraction (XRD) and scanning electron microscopy studies. The details of the impure phases generated during synthesis were obtained from multi-phase Rietveld refinements of XRD data. Experiments revealed that the method of synthesis carried out at 1750?°C involving ZrB₂:B₂O₃:C at a molar ratio of 1:4.5:7.5 could produce highly pure ZrB₂ nano-powders of 67?nm average crystallite size. The magnetometry studies on such pure form of ZrB₂ nano-powders indicated that both paramagnetic and diamagnetic characteristics coexisted in ZrB₂, which could be attributed to its polycrystallinity.     

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.     

Effect of preliminary high-energy ball milling on the structural-phase state and microhardness of Ni3Al samples obtained by spark plasma sintering

The study of the influence of the duration of preliminary high-energy ball milling on the features of the structural-phase state and the level of microhardness of consolidated Ni₃Al samples obtained by the method of spark plasma sintering has been carried out. It was found that the inhomogeneous state of the precursor from the 3Ni-Al powder mixture in the case of preliminary ball milling of a short duration (1 min) is a cause of the formation of an inhomogeneous structural-phase state of the consolidated Ni₃Al sample. An increase in the duration of high-energy ball milling provides a homogeneous phase composition, promotes the refinement of the grain structure and an increase in the microhardness values of the obtained Ni₃Al samples. The main factors determining the processes of structural-phase transformation during the formation of Ni₃Al under the conditions of spark plasma sintering, depending on the preliminary high-energy ball milling, are revealed. It is shown that grain boundary strengthening is the one of the effective mechanisms for increasing the strength of the material under study.     

球磨工艺对B_4C-Al复合粉末性能的影响

利用高能球磨干混的方法制备B4C-Al复合粉末,研究球磨过程中转速、球磨时间对粉末粒度、B4C颗粒均匀性及界面结合的影响。结果表明,球磨转速和球磨时间是影响增强体颗粒分布均匀性以及与基体粉末界面结合的主要因素,存在一个最佳球磨转速和球磨时间使增强体颗粒分布均匀且与基体粉末的界面结合最佳。低转速球磨6h和中转速球磨3h时,增强体颗粒以偏聚的形式分布于基体粉末间隙之间,界面结合率很低。中转速球磨6h时,增强体颗粒均匀地分布于基体材料中,界面结合率较高。中转速球磨12h和高转速球磨6h时,增强体颗粒分布较均匀,界面结合率很高,但是容易形成焊合。     

Optimisation of high energy ball milling parameters to synthesize oxide dispersion strengthened Alloy 617 powder and its characterization

In the present work, ultra-fine powder of oxide dispersion strengthened Alloy 617 was synthesized by high energy ball milling. Milling parameters such as rpm and milling time were varied in the range of 500–2000 and 5–360 min, respectively. Energy applied to the powder in the milling process (Energy per unit mass per hit, E_c) was estimated using the collision model. Effect of milling parameters on the microstructure of powder and refinement of oxides was investigated using X-ray Diffraction (XRD), Scanning electron Microscopy (SEM), conventional Transmission Electron Microscopy (TEM) and High resolution Transmission Electron Microscopy (HRTEM). Desired convoluted lamellar structure with average particle size ∼33 μm was observed during milling at 1000 rpm (E_c ∼ 0.4 kJ/g.hit) for 6 h. TEM analysis of the powder showed the presence of fine oxide dispersoids in the size range 4–16 nm. HRTEM analysis substantiated the presence of fine dispersoids of size ∼4 nm and showed the presence of deformation twins in the matrix. The fine dispersoids in a nanocrystalline matrix is expected to provide superior creep strength to the material at high temperatures.     

高能球磨LaNi5-34%(质量分数)Mg的相组成与热稳定性能

采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、差热分析(DTA)等方法研究了高能球磨及热处理等对新型合金LaNi5-34％(质量分数)Mg的相组成、形貌及热稳定性能等的影响。结果表明：经100r／min球磨100h及190r／min球磨100h后,样品由La、Mg、Ni等非晶。微量的晶体Ni和MgNi2相组成,所得粉末的形状大多为规则的球形或近球形,其颗粒直径范围为0．05～33．0μm。球磨样品具有较好的室温活化特性，其最大电化学放电容量为460mAh／g。该样品经763K保温35d后，得到热稳定性较好的具有纳米尺度的MgNi2、Mg2Ni、Mg2NiLa三相组织，其平均晶粒直径为21.3nm。     

Microstructure,grain growth,and hardness during annealing of nanocrystalline Cu powders synthesized via high energy mechanical milling

In this paper, the microstructure and hardness evolutions of commercially pure Cu subjected to high energy mechanical milling and subsequent annealing treatments in the temperature range of 400–700 °C are investigated. The results demonstrated the simultaneous occurrence of recovery, recrystallization, and grain growth during annealing of the nanocrystalline Cu. The volume fraction of the recrystallized grains estimated using the grain orientation spread exhibits lower values as a result of its dynamic recovery at higher temperatures. The normal grain growth in the range of 400–600 °C and significant abnormal grain growth at higher temperatures are observed during annealing. As a result of the abnormal grain growth, the microhardness value rapidly decreases for the sample annealed at 700 °C. An analysis of the grain growth kinetics using the parabolic equation in the temperature range of 400–600 °C reveals a time exponent of n ≈ 2.7 and an activation energy of 72.93 kJ/mol. The calculated activation energy for the grain growth in the nanocrystalline Cu is slightly less than the activation energy required for the lattice diffusion. This low activation energy results from the high microstrain as well as the Zener-pinning mechanism that arises from the finely dispersed impurities drag effect.