The effects of ball-milling treatment on the densification behavior of ultra-fine tungsten powder

Ultra-fine tungsten powder with a BET particle size of 210 nm was synthesized by sol spray drying, calcination and subsequent hydrogen reduction process. Then this powder was treated by ball-milling, the characteristic changes of this powder before and after milling were investigated. Then the sintering densification behavior of these powders with different ball-milling time (0 h, 5 h, 10 h) were also studied. The results show that ball-milling treatment greatly activates the sintering process of ultra-fine tungsten powder. The relative density of the powder ball-milled for 10 h could reach 97.3% of theoretical density (TD) when sintered at 1900 °C for 2 h, which is 600 °C lower than the required temperature of the traditional micro-scaled powder sintered for the same density. At the same time, ball-milling treatment could substantially reduce the onset temperature of sintering as well as recrystallization, and bulk tungsten materials with more uniform and finer microstructure and much better mechanical properties (hardness) could be obtained.     

烧结方式对CoCrNi中熵合金组织及力学性能的影响

采用机械合金化法（MA）球磨制备CoCrNi中熵合金原料粉末,结合放电等离子烧结（SPS）或高真空烧结制取CoCrNi中熵合金,研究了球磨时间以及退火对CoCrNi中熵合金原料粉末微观形貌、颗粒尺寸及相结构的影响规律,对不同烧结方式制备的合金块体进行微观结构及力学性能研究。结果表明：随着球磨时间的延长,各单质粉末颗粒尺寸不断减小并逐渐融合,在球磨25 h后,原料粉末主要为fcc固溶体结构,还有少量的bcc相;在后续烧结过程中,少量bcc相发生相转变,组织中只有fcc相结构;退火烧结样品的弹性模量为6.57 GPa,是真空烧结的1.55倍,屈服强度为279.28 MPa,与真空烧结后样品的屈服强度相当,退火烧结的延伸率为35.97%,明显大于直接真空烧结;SPS烧结的块体合金表现出高达793.72MPa的屈服强度和61.08%的塑性应变,且维氏硬度(HV)达到3910.2MPa,与其它2种烧结方法相比,SPS在实现高熵合金（HEAs）快速低温烧结方面更具潜力。     

Microstructures and mechanical properties of biocompatible Ti-42 wt.%Nb P/M alloy

Ti-42 wt. %Nb powder was prepared by high-energy mechanical milling (HEMM). The particle size distribution (PSD) of the as-milled powder has been investigated using a particle size distribution analyzer. The morphology and microstructure of the as-milled powder have been investigated by scanning electron microscopy (SEM), X-ray diffractometry (XRD), transmission electron microscopy (TEM), and differential thermal analysis (DTA). Also, the corrosion property and biocompatibility of sintered specimens comprising mixed and milled powders have been investigated. The milled powders were sintered using pulse current activated sintering (PCAS). PCAS was employed in order to provide more refined grain size and full density to Ti-42 %Nb alloy on the basis of short sintering time with pressure. The density of the sintered Ti-42 %Nb specimen fabricated using the milled powder increased with increased milling time due to high free surface area and defect density. The density of the sintered Ti-42 %Nb specimen fabricated using as-mixed powder increased with increased sintering temperature up to 950 °C. The microstructure of the sintered Ti-42 %Nb specimen fabricated using 4h-milled powder was composed of Nb-rich and Nb-poor phases that are more refined and homogeneously distributed. The mechanical properties and biocompatibility of the sintered Ti-42 %Nb specimen fabricated using milled powder were superior to those of a commercial, Ti-6wt.%Al-4wt.%V alloy.     

AlON粉体的合成

以α-Al_2O_3和AlN为原料,利用高温固相反应在氮气气氛下常压合成了AlON粉体.研究了成分配比、合成温度、保温时间对合成AlON粉体含量的影响,并通过热分析测试了合成过程热流和质量的变化.结果表明,当原料Al_2O_3和AlN的质量比为81:18、合成工艺为1750 ℃, 2 h时,得到AlON相的含量达到95%以上.     

高密度纯钨的低温活化烧结工艺及其致密化行为

采用溶胶喷雾干燥-煅烧-氢热还原法制备了BET粒径为0.21μm的超细纯钨粉末,并利用球磨处理进一步活化粉末。研究了超细纯钨粉末形貌及其性能随球磨时间的变化特征,探索了未球磨、球磨5h及球磨10h3种超细纯钨粉末烧结致密工艺,此外还详细研究了纯钨烧结体组织形貌、晶粒尺寸及显微硬度等性能随烧结温度及球磨时间的变化规律。结果表明,球磨处理对超细纯钨粉末的烧结起到了极大的活化作用,由球磨10h粉末制成的压块在1900℃下烧结2h其致密度即可达97.3%,比传统微米级纯钨粉末制成的压块达到相同烧结致密度的温度降低了600℃以上。同时,球磨处理可以大幅降低钨粉的起始烧结温度和再结晶温度,获得组织更加均匀细小、力学性能(硬度)更加优良的钨烧结体。     

The effects of ball-milling treatment on the densification behavior of ultra-fine tungsten powder

Ultra-fine tungsten powder with a BET particle size of 210 nm was synthesized by sol spray drying, calcination and subsequent hydrogen reduction process. Then this powder was treated by ball-milling, the characteristic changes of this powder before and after milling were investigated. Then the sintering densification behavior of these powders with different ball-milling time (0 h, 5 h, 10 h) were also studied. The results show that ball-milling treatment greatly activates the sintering process of ultra-fine tungsten powder. The relative density of the powder ball-milled for 10 h could reach 97.3% of theoretical density (TD) when sintered at 1900 °C for 2 h, which is 600 °C lower than the required temperature of the traditional micro-scaled powder sintered for the same density. At the same time, ball-milling treatment could substantially reduce the onset temperature of sintering as well as recrystallization, and bulk tungsten materials with more uniform and finer microstructure and much better mechanical properties (hardness) could be obtained.     

Effect of Spark-Plasma-Sintering Conditions on Tensile Properties of Aluminum Matrix Composites Reinforced with Multiwalled Carbon Nanotubes (MWCNTs)

In this study, aluminum (Al) matrix composites containing 2 wt.% multiwalled carbon nanotubes (CNTs) were fabricated by powder metallurgy using high-energy ball milling (HEBM), spark plasma sintering (SPS), and subsequent hot extrusion. The effect of SPS conditions on the tensile properties of CNT/Al composites was investigated. The results showed that composites with well-dispersed CNTs and nearly full-density CNT/Al can be obtained. During HEBM, CNTs were shortened, inserted into welded Al powder particles, bonded to Al, and still stable without CNT-Al reaction. After consolidation, Al₄C₃ phases formed in composites under different sintering conditions. With the increase of sintering temperature and holding time, the strength decreased. Conversely, the ductility and toughness noticeably increased. As a result, a good balance between strength (367 MPa in ultimate tensile strength) and ductility (13% in elongation) was achieved in the as-extruded CNT/Al composite sintered at 630°C with a holding time of 300 min.     

Si粉粒径及其添加量对SiC陶瓷材料结构和性能的影响

将平均粒径为75 μm和48 μm、质量分数为0%~8%的Si粉分别添加到SiC陶瓷材料中,在1550℃下保温3 h烧成,研究Si粉粒径及其添加量对SiC陶瓷材料烧结性能、力学性能和显微结构的影响。结果表明:添加不同粒径及质量分数的Si粉可改善SiC陶瓷材料的显微结构,提高其烧结性能和力学性能;在一定范围内,较小粒径的Si粉更有利于形成均匀、致密的SiC烧结体,大幅提升SiC陶瓷材料的性能;当Si粉粒径为48 μm且添加的质量分数为4%时,SiC陶瓷材料的烧结性能和力学性能较优,其体积密度和显气孔率分别为2.58 g/cm3和13.5%,抗弯强度和洛氏硬度分别为25 MPa和115 HRB。      

泡沫铜板与铜粉复合烧结多孔材料的制备

介绍了泡沫铜与铜粉的复合多孔材料松装烧结成形工艺;分别采用SEM观察其几何结构特征和称重法,分析了复合多孔材料的收缩率及孔隙率。结果表明,该材料具有大比表面积、高孔隙率特征;采用与纯铜粉烧结类比的方法,探讨了烧结温度、保温时间及铜粉粒径对复合多孔材料的收缩率和孔隙率的影响。结果显示,相比于铜粉烧结多孔材料,泡沫金属与铜粉烧结复合多孔材料具有更小的收缩率及更大的孔隙率。     

Sinterability and microwave dielectric properties of nano structured 0.95MgTiO3-0.05CaTiO3 synthesised by top down and bottom up approaches

0.95MgTiO₃-0.05CaTiO₃ (MCT) nano powders were synthesised using sol-gel method and high energy ball milling (HEBM). Synthesised powders were characterised using X-ray diffraction analysis to ensure phase purity and HRTEM to determine the fine microstructural features like particle size, interplanar spacing, etc. The powder pellets were heat treated to study the sinterability and microwave dielectric properties and these properties were then compared with the microwave dielectric properties of micron sized sample. Nano powder synthesised using HEBM shows better dielectric properties, sinterability and gets densified to 90% of theoretical density (TD) at 1200 °C/2 h. Dielectric resonators prepared using chemically synthesised nano powder showed poor sinterability and microwave dielectric properties, but, dielectric properties of HEBM samples were very near to that of solid state synthesised samples. Sintered HEBM powders retain the microwave dielectric properties almost to the same level as the solid state synthesised powder with considerable lowering of sintering temperature.     

Rapid Synthesis of V-4Cr-4Ti Alloy/Composite by Field Assisted Sintering Technique

The present investigation deals with synthesis and characterization of V-4Cr-4Ti composite/alloy from unmilled and mechanically alloyed powders. Starting powders were sintered by field assisted sintering technique with varying process parameters viz., temperature, holding time, etc. Both powder and sintered samples were subjected to microstructural and morphological characterization by using scanning electron microscopy and phase analysis was done with the help of X-ray diffraction. Field assisted sintering of unmilled and milled powders has resulted in V-4Cr-4Ti composite and single phase V-4Cr-4Ti alloy. Differential thermal analysis was performed in powder samples to identify the recovery and recrystallization regimes of starting powders. Activation energy of the starting powder was calculated by Kissinger analysis. Field assisted sintering of mechanically alloyed powders resulted in nanostructured single phase V-4Cr-4Ti alloy whereas sintering of unmilled powders resulted in V-4Cr-4Ti composite. X-ray diffraction analysis confirms nanostructured single phase V-4Cr-4Ti alloy after field assisted sintering of milled powders. For identical sintering condition, unmilled V-4Cr-4Ti powders have consumed 75% more current than milled powders. Role of particle size, shape and their distribution on the densification behavior of V-4Cr-4Ti powders are also discussed. Interstitial contamination in the sintered samples were studied using electron probe micro-analysis. Microhardness experiments were done on the sintered samples and their corresponding Hall-Pitch plots were deduced.     

Microstructural characterization and mechanical behaviours of TiN-graphite composites fabricated by spark plasma sintering

The effects of milling time on the particle size distribution (PSD), densification, microstructure, hardness and fracture toughness of spark plasma sintered (SPS) TiN+graphite ceramic were studied. TiN with varying amount of graphite (1, 3, and 5 wt%) were milled at different milling time (8, 24 and 40 h), thereafter sintered at sintering temperature of 1800 °C, holding time of 10 min and pressure of 50 MPa. The relative density and hardness increased as milling time progressed from 24 to 40 h, however, the relative density, hardness, and particle size decreased after 8 h of milling. The microstructural analyses showed that a fully sintered TiN+graphite compact could be achieved at sintering temperature of 1800 °C, with no significant grain growth. Residual stress effect of TiN+5 wt% graphite composite was analyzed using XRD method and the result indicated that there is no significant residual stress on the sample. The relative density, Vickers hardness and fracture toughness of TiN+ 1 wt% Gr, milled for 40 h were 99.24%, 13.90 GPa and 4.0 MPa.m^1/2 respectively.     

Ni/ZrO_2复合材料力学及介电性能研究

采用热压烧结方法,以氧化钇部分稳定氧化锆(Y-PSZ)粉体及不同粒径的金属Ni为原料,制备了Ni/ZrO2复合材料,研究了其力学和介电性能,探讨了烧结过程中Ni形貌的变化对复合材料介电性能的影响.结果表明,随不同粒径Ni粉的掺入,复合材料的抗弯强度减小,且较大粒径的Ni使材料抗弯强度减小更快.随Ni含量增加,复合材料断裂韧性增强.复合材料的介电常数和损耗与Ni粉含量和粒径有关.Ni含量相同时,较大粒径Ni粉的掺入使复合材料具有较高的介电常数和损耗,这是由于在烧结过程中Ni粉形貌发生变化引起的.     

Y2O3-MgO纳米复相红外透明陶瓷制备及其性能研究

以商用Y2O3、MgO纳米粉体为原料,通过球磨混合方法制备了不同Y2O3/MgO配比的Y2O3-MgO纳米复合粉体,使用X射线衍射、扫描电镜、能量色散谱等表征手段对制备粉体的晶体结构、形貌、成分以及均匀性进行了表征。然后采用热压烧结方法制备Y2O3-MgO复相红外透明陶瓷,使用红外光谱仪、维氏硬度计等测试设备对复相透明陶瓷的光学和力学性能进行了分析。重点研究了粉体配比、热压温度、保温和保压时间等关键制备参数对Y2O3-MgO复相红外透明陶瓷晶粒尺度、致密化程度、光学及力学性能的影响。并通过调控粉体制备工艺和热压烧结工艺,制备出了红外透过率达到~80%的Y2O3-MgO复相红外透明陶瓷。同时在Y2O3:Mg0=1:1时,该复相陶瓷的硬度达到了12.3 GPa。     

粉末冶金Nb-35Ti-6Al-5Cr-8V合金组织演变及其力学行为

采用粉末冶金法对不同球磨时间的Nb-35Ti-6Al-5Cr-8V合金机械合金化粉末塑变行为,热压烧结材料的微观组织结构和力学行为进行了研究。研究结果表明：塑性良好的Nb-35Ti-6Al-5Cr-8V粉末随着球磨时间增加首先变形为大尺寸的片状、后经持续的加工硬化破碎成絮状;热压烧结能够制备微观组织可控晶粒细化的Nb-35Ti-6Al-5Cr-8V合金,合金由单一的Nbss相构成,Ti、Al、Cr、V元素固溶引起Nb晶格尺寸减小0.0685 ?;随着球磨时间增加合金晶粒明显细化进而显著提高了合金的维氏硬度和室温压缩强度,其变化符合材料硬度和强度的Hall-Petch规律。粉末冶金制备Nb-35Ti-6Al-5Cr-8V合金的各项力学性能明显优于熔铸法制备合金。     

Mechanical properties of molybdenum products prepared by using molybdenum powders with different micro-morphologies

Using two kinds of molybdenum(Mo) powders with different micro-morphologies as raw materials, the Mo wires with a diameter of 0.18 mm and Mo sheets with thickness of 0.5 and 0.2 mm were prepared at the same process of pressing, sintering, drawing, or rolling, respectively. By comparative analysis on the microstructure and mechanical properties of Mo wires and Mo sheets, the effect of Mo powder micro-morphology on properties and quality of Mo products was studied. The results show that,compared with that prepared by traditional Mo powder with inhomogeneous particle size and aggregation, the Mo wires prepared by specific Mo powder with homogeneous particle sizes, less agglomeration, and better dispersion exhibit higher yield, higher tensile strength, and lower elongation at room temperature, and the Mo sheets also show excellent high-temperature performances and better isotropy. The essential reason for those is the difference of Mo powder micro-morphology. Inhomogeneous particle size and aggregation of Mo powder greatly influence the microstructure of Mo sintered compacts and mechanical properties of Mo products.     

球磨工艺和分散剂对陶瓷结合剂粉体解团聚的影响

通过球磨工艺和添加分散剂相结合的方法对陶瓷结合剂团聚体进行解团聚,研究球磨参数和分散剂添加量对解团聚效果及结合剂机械性能的影响,并用激光粒度分析仪、SEM、万能材料试验机测试结合剂粉体解团聚前后的粒度、显微形貌、抗折强度。结果表明:采用小粒径(5 mm)的磨球,添加质量分数为2.5%的分散剂球磨2 h后,结合剂粉体分散性良好,基本没有团聚现象,其D₅₀可降至0.186 μm,且球磨后的粉体在700 ℃烧结后,其抗折强度达到26.2 MPa,比原始团聚体烧结后样品的强度提升了近45%。      

超细WC-Co硬质合金的制备与性能研究

利用高能球磨法制备纳米级WC-Co混合粉末,采用脉冲电流烧结技术进行烧结。用能谱分析仪(EDX)对球磨后的粉末进行成分分析,用X射线衍射(XRD)对比分析球磨前后WC-Co混合粉末的衍射峰变化,用透射电子显微镜(TEM)和扫描电子显微镜(SEM)对所制备的粉末及烧结材料进行了组织形貌观察,并测定了烧结试样的硬度。结果表明:随着球磨时间的延长,WC-Co纳米粉末的粒度逐渐变小,当球磨时间超过30h后获得了粒度为100nm以下的WC-Co纳米粉末。脉冲电流烧结后获得超细WC-Co硬质合金,与传统的WC-Co硬质合金相比,超细WC-Co硬质合金具有更高的硬度(HRA92.5～94)和耐磨性。另外通过实验获得了最佳的烧结工艺参数。     

超细硬质合金中晶粒非均匀长大机理

采用市售的粒度为0.8μm的WC粉末和粒度为1.6μm的Co粉制备了WC-10%Co超细硬质合金,通过金相显微镜﹑扫描电子显微镜观察了不同烧结温度下制备的试样WC晶粒形貌,对超细晶粒硬质合金非均匀长大现象及机理进行了研究。结果表明:粉末湿磨后的粗大颗粒在烧结过程中起晶核作用,是引起晶粒非均匀长大的关键因素。固相烧结时,烧结体中细小颗粒受到张力的作用发生旋转,当其取向与邻近的大颗粒取向一致时,形成共格界面,以粗大晶粒为核心以并合的方式非均匀长大;液相烧结时,细小晶粒溶解并优先地在大晶粒的某些低能量晶面如(0001)和(1010)面析出,引起晶粒异常长大。本研究中,当烧结温度达到1 410℃时,WC晶粒可异常长大为接近20μm的粗大晶粒。     

Effects of silver powder particle size on the microstructure and properties of Ag-Yb<Subscript>2</Subscript>O<Subscript>3</Subscript> electrical contact materials prepared by spark plasma sintering

Ag-Yb₂O₃ electrical contact materials were fabricated by spark plasma sintering (SPS). The effects of silver powder particle size on the microstructure and properties of the samples were investigated. The surface morphologies of the sintered samples were examined by optical microscope (OM), and the fracture morphologies were observed by scanning electron microscopy (SEM). The physical and mechanical properties such as density, electrical resistivity, microhardness, and tensile strength were also tested. The results show that the silver powder particle size has evident effects on the sintered materials. Comparing with coarse silver powder (5 μm), homogeneous and fine microstructure was obtained by fine silver powder (≤0.5 μm). At the same time, the electrical conductivity, microhardness, and tensile strength of the sintered samples with fine silver powder were higher than those of the samples with coarse silver powder. However, silver powder particle size has little influence on the relative densities, which of all samples (both by fine and coarse silver powders) is more than 95%. The fracture characteristics are ductile.