高能球磨制备纳米WC-Co复合粉末及其SPS烧结

本文采用高能球磨法制备纳米结构WC-Co粉末,并采用放电等离子体烧结方法(SPS)对该纳米粉末进行致密化。使用X射线衍射、SEM等手段分析了高能球磨对WC-Co复合粉末中WC晶粒尺寸和粒度的影响。发现经过90h左右的高能球磨,WC-Co的粉末粒度可以达到300nm左右,而WC的晶粒尺寸可以细化到8nm左右。经过SPS烧结后,合金中的WC相的晶粒尺寸可以保持在300nm左右,而Co多以fcc结构出现。     

高能球磨法制备纳米晶Ni粉的研究

采用高能球磨法制备出了纳米晶镍粉,并利用X射线衍射仪（XRD）、扫描电镜（SEM）、透射电镜（TEM）等分析检测手段,研究了该纳米晶镍粉末的结构、形貌和相的变化。结果表明,镍粉末平均粒度和晶粒度随球磨时间增加不断减小,而应变随球磨时间增加不断增大;当高能球磨54h后,球磨产物为FCC结构的鳞片状多晶体,晶粒度为17nm左右,应变为0.48%,颗粒尺寸为150～200nm;球磨时间增加至98h,产物中出现非晶相,但仍以多晶为主,晶粒尺寸为7nm,应变为1.24%,粉末团聚严重。     

Preparation of WC nanoparticles by twice ball milling

In order to improve the ball milling efficiency of WC powders and thus to fabricate nano-grained WC–Co cemented carbides with high mechanical properties, WC nanoparticles were prepared by twice ball milling in nylon vessels. The best technology to disperse WC powders in alcohol was investigated at first. Based on the dispersion results, 2 wt.% PEG was used with La₂O₃ as additive to improve ball milling efficiency. The particle size, crystal structure, surface morphology and surface properties were tested by a laser particle sizer, XRD, FE-SEM and FT-IR, respectively. During the first ball milling, sample d achieved the best milling performance, including average particle size (168 nm) and grain size (27.2 nm) among samples a (pure WC), b (with PEG), c (with La₂O₃) and d (with PEG and La₂O₃). La₂O₃ could greatly decrease particle size and grain size while PEG could narrow particle size distribution. During the second milling, the particle size and grain size of sample d reached 89 nm and 13.2 nm at 96 h, respectively. The results indicated that twice ball milling can greatly improve particle size and grain size compared with the first ball milling, and further narrow the size distribution. In conclusion, multiple ball milling can reduce the particle size of certain powders with suitable milling technology.     

PREPARING NANO-CRYSTALLINE La DOPED WC/Co POWDER BY HIGH ENERGY BALL MILLING

The La doped WC/Co powder was prepared by high energy ball milling. The changes of crystal structure, micrograph and defect of the powder were investigated by means of XRD (X-ray diffraction), SEM (scanning electron microscope) and DTA (differential thermal analysis). The results show that adding trace La element into carbides is effective to minish the grain size of WC/Co powder. The La doped carbides powder with grain size of 30nm can be obtained after 10h ball milling. The XRD peak of Co phase disappeared after 20h ball milling, which indicated solid solution (or secondary solid solution) of Co phase in WC phase. The La doped powder with grain size of 10nm is obtained after 30h ball milling. A peak of heat release at the temperature of 470℃ was emerged in DTA curve within the range of heating temperature, which showed that the crystal structure relaxation of the powder appeared in the process of high energy ball milling. After consolidated the La doped WC/Co alloy by high energy ball milling exhibits     

Ultramicro molybdenum nitride powder prepared using high-energy mechanochemical method

Using the specially designed mechanochemical ball-mill equipment, ultramicro molybdenum nitride powders were prepared from pure molybdenum powders in ammonia atmosphere at room temperature by high-energy ball milling. The structure and the particle size of the powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The results show that the mass ratio of grinding media to powder was 8:1, after milling for 30h the Mo2N of fcc structure was obtained, and the average particle size of the powders was around 100 nm. It is found that the chemisorption of ammonia onto the fresh molybdenum surfaces created by milling was the predominant process during solid-gas reaction, and the energy input due to introduction of highly dense grain boundaries and lattice defects offered the activation energy for the transition from Mo-N chemisorption to molybdenum nitride. In addition, the change of Mo electronic undersaturation induced by the grain refining accelerated the bonding between Mo and N. The mechanism model of whole nitriding reaction was given. During the high-energy ball milling processing, the rotational speed of milling played a critical role in determining the overall reaction speed.     

Cr_3C_2粉体的高能球磨细化

采用高能球磨工艺对Cr3C2粉末进行研磨。研究了粉体粒度随球磨时间的变化。结果表明:随着球磨时间的增加,粉体粒度不断细化,最后BET粒度趋于稳定在50nm左右。Cr3C2粉末高能球磨细化机理是:机械力通过破碎一次颗粒间的烧结颈,并不断细化粉末,Cr3C2粉末的最终粒度取决于一次颗粒的晶粒尺寸;长时间球磨不能进一步细化粉末反而容易形成新的团聚体。     

高能球磨制备纳米TiC粉末

应用高能球磨机,用Ti和C粉末在室温下全盛了纳米级TiC晶粒,并对合成后的粉末进行了微观组织分析,实验结果表明：用机械合金化（MA）法可以在比较短的时间内合成TiC粉末,其合成机理为机械碰撞诱发的自蔓延反应机理,经过球磨反应可以得到平均颗粒大小为5.641um,并且具有10nm左右的纳米晶粒TiC粉末,DAT分析表明,利用加热方法合成TiC必须在636.5℃以上才能进行,而通过球磨工艺可以使该合成过程在室温下进行。     

Preparing nano-crystalline rare earth doped WC/Co powder by high energy ball milling

The nano-crystalline rare earth doped WC/Co powder was prepared by high energy ball milling. The nano-crystalline powders were characterized by means of XRD (X-ray diffraction), SEM (scanning electron microscope) and DTA (differential thermal analysis). The results show that adding trace rare earth elements into carbides is effective to minish the grain size of WC/Co powder. The grain size of rare earth doped powder became two times smaller as compared with the undoped powder within ball milling times of 25–45 h. The XRD peak of Co phase disappeared after 25 h ball milling. A sharp peak of heat release at the temperature of 597 °C was emerged in DTA curve within the range of heating temperature. After consolidated the rare earth doped WC/Co alloy by high energy ball milling exhibits ultra-fine grain sizes and better mechanical properties.     

纳米复合银基电触头材料的研究

利用高能球磨技术及热压烧结工艺制备出第二相弥散均匀分布于Ag基体中的纳米复合AgNi和AgSnO2触头，对复合粉末和合金触头进行了X射线衍射(XRD)、扫描电镜(SEM)和透射电镜(TEM)分析。结果发现：经长时间高能球磨后，复合粉末的晶粒明显细化，第二相粒子尺寸已达到40nm左右，并在球磨过程中通过嵌入、焊合弥散分布于Ag基体中，消除了传统方法第二相聚集及在晶界处的连续析出等缺陷。在退火、热压过程中第二相并未明显长大，仍保持在50nm左右。对触头进行SEM观察时发现，2种触头的晶界处都保持着有利于电性能的Ag膜。与常规商用触头相比，纳米复合触头有分散电弧作用，表面没有明显的熔池和液体喷溅，呈现出较好的耐电弧侵蚀特性。     

高能球磨制备Al-Pb-Si-Sn-Cu纳米晶粉末的特性

通过机械合金化制备了Al-15％Pb-4％Si-1％Sn-1．5％Cu(质量分数)纳米晶粉末。采用X射线衍射(XRD)，扫描电镜(SEM)和透射电镜(TEM)对不同球磨时间的混合粉末的组织结构、晶粒大小、微观形貌以及颗粒中化学成分分布情况进行了研究。结果表明混合粉末经过球磨后形成了纳米晶，其组织非常均匀。球磨对Pb的作用效果明显大于对Al的作用效果，经过40h球磨后Pb粒子达到40nm，而Al在球磨60h后晶粒为65nm；经球磨后，Cu和Si固溶于Al的晶格中，而Sn则固溶于Pb晶格中，并且Al和Pb发生了互溶，形成了Pb(Al）超饱和固溶体；在球磨过程中硬度高的脆性粒子Si难于完全实现合金化。     

粗晶和纳米晶FeAs的微观结构与磁学性能

研究粗晶及纳米晶FeAs的微观结构和磁学性能.首先通过高能球磨和热处理制备粗晶FeAs,随后将粗晶FeAs进行不同时间球磨得到纳米晶FeAs.结果表明,球磨时间为32 h时,平均晶粒尺寸由>100 nm减小到32.4 nm,同时内应变增加到0.568％.随着球磨时间的增加,矫顽力由球磨前的29.2 kA/m降低到15....     

低温球磨和真空热压技术制备的纳米晶纯铝块体的强化机理

利用液氮球磨和真空热压技术制备了纳米晶纯铝块体材料。采用X射线衍射(XRD)、扫描电镜(SEM)和透射电镜(TEM)对材料的晶粒尺寸和微观组织进行研究,分析了影响热稳定性的因素和强化机理。研究表明,液氮球磨以后材料晶粒尺寸为37nm,经过真空热压和热挤压后晶粒有所长大,晶粒大小约300nm,纳米晶结构基本得到保持。分析晶粒热稳定性的原因在于球磨过程中生成的AlN等粒子的晶界钉扎以及引入的杂质溶质的拖拽作用。纳米晶纯铝块体的拉伸强度极限σb为173MPa,伸长率fε为17.5%。     

Microstructure and magnetic properties of Co/Al2O3 nanocomposite powders

Nanocomposite powders of magnetic cobalt nanoparticles dispersed by nonmagnetic Al₂O₃ particles have been prepared by planetary ball milling. Ball milling of the CoO and Al mixture powder after a certain milling duration reduces CoO to (fcc and hcp) Co completely and oxidizes Al to -Al₂O₃ simultaneously. The average grain sizes of the nanocomposite powders are 19 nm for Co and 28 nm for -Al₂O₃ after the completion of the reduction reaction. By direct ball milling of the mixture of Co and Al₂O₃, the allotropic phase transformation of Co was observed and the average grain size of Co is reduced to 5 nm. For both the samples of the mechanochemical series and the direct milling series, the saturation magnetizations of the nanocomposite powders decrease with decreasing average grain size of Co. This may be due to the enhancement of the interface effects and the increase of the superparamagnetic particles with decreasing Co grain size. The coercivities of the Co/Al₂O₃ nanocomposite powders increase up to 380 Oe. The increasing grain boundaries with decreasing Co grain size result in the domain wall pinning which predicts the coercivity enhancement. In addition to the grain size effects, the reduction of the particle size toward the size region of single domain also contributes to the increase of coercivity.     

EFFECT OF MILLING INTENSITY ON STRUCTURAL CHANGES OF MIXED Al－Fe－Ni POWDERS IN MECHANICAL ALLOYING PROCESS

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Refinement process and mechanisms of tungsten powder by high energy ball milling

The grain refinement process and mechanisms of tungsten powder during ball milling are explored based on different ball milling time. From the results of scanning electron microscopy (SEM), the model for ball milling process is proposed to include four stages: welding stage, squeezing stage, fracturing stage and dynamic balance stage. Microstructure of tungsten powder examined by transmission electron microscopy (TEM) shows that the tungsten powder ball milled for 50 h has polycrystalline grains and most of them have long strip structure with high angle grain boundaries. Nanocrystalline tungsten powder with minimum grain size of 5 nm was obtained in the final stage of ball milling.     

Properties of WC–8Co hardmetals with plate-like WC grains prepared by plasma-assisted milling

WC-8C0 hardmetals with different proportions of prismatic WC grains and plate-like WC grains were directly produced through sintering the W-C-8C0 elemental powder mixture which was fabricated by dielectric barrier discharge plasma(DBDP)-assisted milling.The morphology of prepared WC-8C0 hardmetals,geometry and the preferential orientation of plate-like WC were investigated by X-ray diffraction(XRD) and scanning electron microscopy(SEM) analysis.The results demonstrate that the microstructure and mechanical properties of the sintered hardmetals are related to the morphology of W grain which is dependent on DBDP-milling time.The DBDP for 1 h(DBDP-1 h)-milled W-C-Co powder contains granular W particles that tend to form prismatic WC grains,while the DBDP for 3 h(DBDP-3 h)-milled powder contains lamellar W particles that generate plate-like WC grains.By adjusting the weight ratio of DBDP-1 h powder and DBDP-3 h powder in W-C-8C0 mixture,the proportion of plate-like WC in the hardmetals can be controlled,and relatively high transverse rupture strength(TRS) is obtained as the proportion of plate-like WC grain in the hardmetals is about 35%in present experimental condition.     

Changes in the microstructure and hydrogen storage properties of Ti-Cr-V alloys by ball milling and heat treatment

Changes in the microstructure and hydrogen storage properties of Ti-Cr-V alloys were investigated after a combination of ball milling and heat treatment. Two different sets of balls and vials made of tungsten carbide (WC) and stainless steel (STS) were used for milling the samples. Ball milling using WC balls and vials induced WC contamination, and it caused compositional changes in the matrix during heat treatment. When STS balls and vials were used, meanwhile, no peak of the second phase caused by contamination was found in the X-ray diffraction (XRD) data. In the case of the sample that completed only the milling process, the crystallite size calculated from the XRD data, 20-30 nm, agreed well with the grain size obtained from transmission electron microscopy (TEM). On the other hand, for the sample that was heat treated after milling, the strain decreased from 0.74% to 0.18%, the crystallite size increased to 70-80 nm, and the grain size grew up to the level of hundreds of nanometers. The changes in microstructure induced by the ball milling and heat treatment influenced the hydrogen storage properties, such as plateau pressure, hysteresis, and phase transformation with hydrogen absorption. Thus, the relationship between the microstructure and hydrogen storage properties can be explained.     

固化球磨纳米晶粉末制备块体超细晶Mg-3Al-Zn合金(英文)

采用粉末冶金技术制备块体超细晶Mg-3Al-Zn合金。首先采用球磨Mg、Al、Zn混合粉末来制备纳米晶粉末,所得的粉末的平均晶粒尺寸为45nm。随后将球磨好的粉末封入铝包套内,分别在室温和633K温度下,在真空烧结炉内进行真空热压。然后将烧结后的样品在423K下挤压以进行进一步的致密化处理。结果表明:致密后的冷压样品的晶粒尺寸为180nm,而热压坯的晶粒尺寸为600nm,冷压样品的屈服强度达464MPa;超细晶镁合金的强化机制主要是细晶强化,这主要是由于HCP结构的材料晶粒尺寸对材料的影响更为明显。固化后冷压样品的最终密度为(1.777±0.006)g/cm3,而热压样品的最终密度为(1.800±0.006)g/cm3。     

高能球磨过程中Ti与BN的反应

通过研究高能球磨工艺制备纳米复合粉体过程中Ti与BN的反应过程和机理,对所制备粉体的显微结构进行了表征．实验结果表明,采用金属Ti和BN为原料,球磨10h后,即形成球状纳米复合粉体,其中球状粉体颗粒的尺寸在随后的球磨过程中基本保持不变．BN由于球磨而发生解理进而包裹Ti颗粒可能是形成稳定的球状纳米颗粒的原因．球磨30h后,Ti与BN开始反应生成TiN．TiN纳米粒子与未反应的Ti,B和BN共同形成平均粒径约100nm的、较均匀分布的球状纳米复合粉体．     

Mechanical alloying of platinum with 5% ZrO2 nanoparticles for glass making tools

Synthesis and characterization of mechanically alloyed Pt–5%ZrO₂ (volume fraction) for structural components in the glass industry were described. Zirconia (ZrO₂) nanoparticles (<100 nm) were produced by the electrical explosion of zirconium (Zr) wires, and blended with platinum (Pt) powders (<44 μm) for 2–72 h in ambient atmosphere. The Pt particle size followed the typical decreasing trend of the normal ball milling process up to 48 h, but particle agglomeration was observed at 72 h. The grain size evolution was similar to that of the particle size, dropping down to around 50 nm at 48 h. The root mean square strain of the Pt crystallites showed the opposite behavior, maximizing at 48 h with a subsequent relaxation process. For the 48 h ball milled powders, spark plasma sintering was carried out to form a bulk disk. The measured mass loss of the sintered bulk sample shows a decent thermal stability despite its relatively low density.