粒度可控氧化钇粉体的制备

以硝酸钇为原料溶液,采用氨水-草酸2步沉淀法合成了中心粒径（D₅₀）为1.00~2.00 μm的氧化钇粉体,粉体分散性好,粒度可控.考察了沉淀剂的浓度、物料的浓度、反应温度、加料速度以及pH值等因素对氧化钇粉末中心粒度的影响.采用激光粒度仪、比表面仪、扫描电子显微镜等仪器对实验过程及实验结果进行表征和分析.结果表明,在氨水浓度为1.0 mol/L、草酸质量浓度为10 %、滴加速度为20 mL/min、草酸溶液温度为80 ℃、氨水沉淀后pH值在7~8之间、草酸转化后pH值小于1的条件下,可通过调节硝酸钇的浓度在0.4~0.8 mol/L之间,以制备中心粒径（D₅₀）在1.00~2.00 μm范围内、比表面积在3.2~13.3 m2/g之间的氧化钇粉体.      

利用冶金含铁粉尘制备超细铁粉的试验

针对冶金含铁粉尘杂质含量较高、原始颗粒细小容易污染环境等问题，采取除杂提纯分离- 还原两步法制备超细铁粉。通过湿法反应、磁选、浮选等除杂提纯工序，含铁粉尘中SiO2质量分数降低到0.12%，CaO、MgO质量分数同时得到不同程度的下降。分离杂质后的含铁粉尘还原试验结果表明，在H2气氛、还原温度为750 ℃、保温1 h的条件下，得到的超细铁粉TFe质量分数达到99.27%，微观形貌观测颗粒平均粒径约为1 μm，比表面积为2.495 m2/g。经过压制成型及烧结试验，表明得到的超细铁粉易于压制成型，颗粒烧结反应活性好，压制的成型坯体烧结温度为850～900 ℃，明显优于常规还原铁粉。     

超细铁粉的制备及其对硝酸盐的降解

分别采用液相还原改性法和微乳液法制备超细铁颗粒,用乙醇-水体系制备镍包覆铁颗粒的Fe/Ni双金属颗粒,用来进行硝酸盐的降解实验,并用扫描电镜(SEM)和X射线衍射(XRD)分析超细粉末的物相结构及形貌.结果表明:通过液相还原改性法制备的超细铁粉,颗粒形状不规则,颗粒大小在0.2～0.3 μm之间;而用乙醇-水体系制备的铁/镍粉颗粒为等轴晶粒,颗粒大小也在0.2～0.3 μm之间;加入PEG-6000可改善液相改性法和醇-水法制备的铁粉的分散性.微乳液法制备的铁粉为球形颗粒,存在较明显的团聚现象,颗粒大小在0.5～ 1μm之间.在相同条件下,不同方法制备的超细铁粉降解硝酸盐的能力由高到低依次为:微乳液法制备的铁粉＞乙醇-水体系法制备的Fe/Ni双金属粉＞液相还原改性制备的铁粉＞不加PEG的乙醇-水体系制备的铁粉.     

Spheroidization of Iron Powder in Microwave and Hybrid Plasma Torches

The process of porous iron powder spheroidization with a particle size from 45 to 85 μm is investigated in the microwave discharge and joint microwave and DC discharge modes in nitrogen and helium plasma. The powder was prepared by air spraying and annealed in hydrogen. Spraying in plasma results in hollow spheroidized particles with a wall thickness from 1 to 10 μm. The fraction of spheroidized powder particles in their total number is determined. It is revealed that the degree of spheroidization of iron powder particles linearly increases with an increase in the microwave radiation power from 1.5 to 5 kW. The combination of operational conditions of the microwave radiation with the arc discharge is observed when using the hybrid plasmatron mode, which makes it possible to increase the plasma temperature. An almost 100% spheroidization of iron powder is attained with the power ratio of microwave and arc discharges of 1 : 1. The metallographic investigation of spheroidized particles showed that their finite size differs from the initial one approximately tenfold. It is established that, irrespective of the spheroidization mode, the iron powder oxidizes, which is caused by an insufficient degree of purification of plasma-forming gases. The structure of the particle surface when using nitrogen or helium as a plasma-forming gas is different. The experiments show that the application of helium is preferential because the particles have only insignificant roughness in this case when compared with the particle structure when performing spheroidization with the use of nitrogen.

     

六偏磷酸钠对磁性复合流体分散性及光学玻璃抛光性能的影响

为了提高磁性复合流体(Magnetic Compound Fluid,MCF)的抛光性能,通过实验调查无机电解质分散剂六偏磷酸钠(Sodium Hexametaphosphate,SHMP)对MCF颗粒团聚的影响,研究MCF抛光液颗粒分散性与BK7光学玻璃抛光材料去除率和表面粗糙度的变化关系。在MCF中添加不同质量分数的SHMP,测试MCF中颗粒的粒径分布和中值粒径D50的变化,并采用扫描电镜观察MCF中颗粒分散性;利用不同含量SHMP的MCF对BK7光学玻璃进行抛光加工,研究SHMP含量变化对光学玻璃抛光材料去除率和表面粗糙度的影响规律。实验表明,在MCF中添加适量SHMP能够减少抛光液颗粒的团聚,提高MCF抛光液的颗粒分散性,改善BK7光学玻璃的材料去除率和表面质量。当SHMP质量分数为3%时,中值粒径D50达到最小值7.023μm,并且MCF抛光液的分散性最佳,材料去除率达到最大值22.6×10^-4 g/min,表面粗糙度达到最小值15.78 nm。     

Effect of scandia on tungsten oxide powder reduction process

Scandia doped tungsten powders were prepared by spray drying combined with two-step hydrogen reduction. The particle size of doped tungsten powder, powder morphology and doped tungsten matrix were characterized by scanning electron microscope, X-ray diffraction and laser diffraction particle size analyzer, respectively. The reduction behavior of Sc₂O₃ doped tungsten oxide and the effect of Sc₂O₃ on the property of tungsten powder were studied by the temperature programmed reduction. The experimental results showed that the precursor powders prepared by spray drying had spherical shape. The addition of Sc₂O₃ could decrease the reduction temperature of tungsten oxide. The scandia doped tungsten powder had sub-micrometer size in the range of 0.1 to1 μm and scandium distributed evenly in the powder. By using this kind powder, sub-microstructure cathode matrices with semispherical grains and homogenous distribution of scandium were obtained.     

Transient liquid phase sintering of high density Fe3Al using Fe and Fe2Al5/FeAl2 powders Part 1: Experimentation and results

Abstract

High density Fe₃Al was produced through transient liquid phase sintering, using rapid heating rates of greater than 150 K min^-1 and a mixture of prealloyed and elemental powders. Prealloyed Fe₂Al₅/FeAl₂ (50Fe/50Al, wt-%) powder was added to elemental iron powder in a ratio appropriate for producing an overall Fe₃Al (13·87 wt-%) ratio. The heating rate, sintering time, sintering temperature, green density and powder particle size were controlled during the study. Heating rate, sintering time and powder particle size had the most significant influence upon the sintered density of the compacts. The highest sintered density of 6·12 Mg m^-3 (92% of the theoretical density for Fe3Al) was achieved after 15 minutes of sintering at 1350°C, using a 250 K min^{- 1} heating rate, 1-6 μm Fe powders and 5·66 μm alloy powders.

SEM microscopy suggests that agglomerated Fe₂Al₅/ FeAl₂ particles, which form a liquid during sintering, are responsible for a significant portion of the remaining porosity in high sintered density compacts, creating stable pores, larger than 100 μm diameter, after melting. High density was achieved by minimising the Kirkendall porosity formed during heating by unbalanced diffusion and solubility between the iron and Fe₂Al₅/FeAl₂ components. The lower diffusion rate of aluminium in the prealloyed powder into the iron compared with elemental aluminium in iron, coupled with a fast heating rate, is expected to permit minimal iron-aluminium interdiffusion during heating so that when a liquid forms the aluminium dissolves in the iron to promote solidification at a lower aluminium content. This leads to a further reduction in porosity.     

含氟铈基稀土抛光粉的制备及其抛光性能

以碳酸镧铈为前驱体,采用氢氟酸氟化、高温焙烧、机械搅拌磨的方法制备中位粒径较小的含氟铈基稀土抛光粉。结果表明,所得产物中固溶体具有立方萤石结构;随着氟掺杂量的增加,开始析出四方结构的LaOF相,CeO2的XRD特征峰向右偏移,结晶度提高,粉体的振实密度随之增大;对光学玻璃的抛光能力在氟掺杂量为6%时出现极大值,被抛光物体的表面光洁度随氟掺杂量的增大而下降。     

碳酸氢铵沉淀法制备氧化铈抛光粉

利用碳酸氢铵做沉淀剂制备氧化铈抛光粉,通过L16(44)正交试验,研究了温度、硝酸铈浓度、滴加速度和搅拌速度对氧化铈粒度和比表面积的影响。得到的最佳粒度制备工艺条件为:温度60℃、硝酸铈浓度50g/L、搅拌速率500r/min、滴加速度50mL/min。并对最佳制备工艺条件下制取的抛光粉进行粒度、形貌和抛蚀量进行研究。     

Al-Ni-Co微细球形粉末的制备及SLM成形研究

采用气雾化(IGA)制备了Al-Ni-Co粉末,初筛后的最大粉末粒径小于150μm。分别采用霍尔流速计、XRD、SEM、VSM等测试方法研究了不同粒径范围Al-Ni-Co微粉的微观形貌、相成分、磁性能等。研究表明：微粉的球化率在95%左右;50～80μm范围微粉的流动性相对最好;20μm以下微粉因为粒径偏小,成分偏析较为严重;80～150μm微粉因为粒径过大,表面吸附卫星小颗粒,粗糙度较差;Al-Ni-Co微粉的磁性为软磁,相组成为AlNi和FeCo相。综合比较微观结构、相成分及粉末占比量,选取20～80μm的Al-Ni-Co微粉采用SLM法制备了6组Al-Ni-Co圆柱形磁体,热处理后磁体的密度、磁性等综合性能达到铸造Al-Ni-Co磁体的性能水平。     

Microshear banding in shock-consolidated microcrystalline alloy powders

Microshear bands (<0.02–0.03 μm thick), formed as a result of inhomogeneous plastic deformation within heavily deformed powder particle interiors, are observed during shock consolidation of microcrystalline Markomet 1064 (Ni_55.8 Mo_25.7 Cr_9.7 B_8.8), and nickel based superalloys Pyromet 718 and Rene 95. Although part of the shock energy is utilized in melting of particle surfaces due to preferential plastic deformation near interfaces, a nonnegligible amount of energy is dissipated in plastic deformation within particle interiors. This involves localized regions of shear which are manifested as fine microshear bands of heavily twinned material, confined within individual powder particles. The thickness and length of the microshear bands is more than several orders of magnitude smaller than that in the macroscopic bands observed in materials subjected to unconstrained high-strain-rate deformation. The small size of the shear bands is attributed to the fact that the particle strain is limited, as individual powder particles are deformed to conform to their neighbors in the shock consolidation process.     

Sintering of aluminum powders in air in the presence of silumin and KAlF<Subscript>4</Subscript> flux: Model experiments

The role of a KAlF₄ flux and the effect of its particle size on the sintering process of a PA-4 aluminum powder are investigated. A dispersed flux is more effective. In model experiments, the mechanisms of flux spreading over the surface of aluminum are established. On sintering an aluminum powder of particle size d > 60 μm, it is recommended to use a flux with particle size d < 50 μm at its total content of 1–3%.     

磁流变抛光液的研制、表征及使用

针对现有抛光技术的不足,研究将磨料颗粒包覆在铁磁性颗粒表面,制备出磨料颗粒与铁磁性颗粒的复合粒子,并由此制备磁流变抛光液。通过扫描电镜观察,表明磨料较为均匀地包覆于铁磁性颗粒表面;利用流变仪测试磁流变抛光液的流变性,当磁场为0.8 T、剪切速率为100 s-1时,剪切应力达到45 kPa。通过智能磁流变抛光机对两款316L材质的金属粉末注射成形冷饮机配件进行抛光实验,验证磁流变抛光液的抛光效果,结果表明,抛光后粉末注射成形配件的表面粗糙度明显下降,说明所研制的磁流变抛光液对于粉末冶金制品表面粗糙度具有较高的去除率。     

Mechanical properties of metal injection moulded 316L stainless steel using both prealloy and master alloy techniques

Abstract

Stainless steel 316L MIM components can be made from either prealloyed powders or from master alloys blended with carbonyl iron powder. In this study these two techniques were compared using prealloyed and master alloyed gas atomised powders of ? 16 μm and ? 22 μm sizes. Four different compounds were prepared, characterised and injection moulded into tensile bars. The bars were compared for green strength, green defects, sintered strength and microstructure. The green components are stronger when carbonyl iron powder is used with the gas atomised master alloy. This material also seems to be less susceptible to moulding defects. The sintering strength of the material produced using the pre-alloyed powder was higher than the master alloyed prepared material. Little difference in mechanical properties existed between the materials fabricated from gas atomised prealloyed ? 16 μm and the ? 22 μm powders. Also, the viscosity of the mixtures was higher for the ? 16 μm material and the master alloy mixtures than for the –22 μm gas atomised prealloyed powders.     

EPMA drives collaborative development projects

Abstract

An analysis has been performed on the selective removal of particles from the edges and thin lands on green iron powder compacts. The voids created as a result of this ‘picking’ are believed to be due to large (+ 125 μm (+ 120 mesh)) particles in the iron powder mix. Microscopic examinations indicated that in all cases picking occurred within isolated regions of large pore and particle size. Two possible independent causes for this problem have been advanced: segregation of large particles within the feed shoe during die filling; and an uneven load distribution across the face of a part due to the presence of tooling impressions on the upper punch. A series of follow up tests showed no change in the relative position of the large pore size region with upper punch orientation. Therefore, by deduction, particle segregation is advanced as the main cause of the observed picking. Suggestions are presented to alleviate this problem. PM/0495     

Magnetic Properties of Nanocrystalline Powder Cores Fabricated by Mechanically Crushed Powders

Fe73.5Cu1Nb3Si15.5B7 nanocrystalline powder cores with different particle sizes ranging from 10 to 125μm were fabricated by cold-pressing techniques.The cores exhibited increased core loss Pcvand decreased initial permeabilityμiwith addition of fine powders below 50μm in size,and the content should be less than 40mass%.It was thought to be closely related to the high coercive force Hcdue to the stresses generated during the crushing process and high demagnetization fields of small powders.Furthermore,modifying the alloy compositions by adding defined amount of Ni could improve the soft magnetic properties,including superior characteristics of permeability under high direct current(DC)bias field and comparable low core loss at high frequency.     

TiO2/Mg（OH）2新型抗菌阻燃复合材料的研究

采用氨气鼓泡法制备TiO2/Mg(OH)2多功能复合材料,其中以钛酸正丁酯为前躯体,硝酸铵和九水硝酸铁为氮、铁掺杂源,利用水热法制备了氮、铁共掺杂TiO2粉体。通过XRD、FE-SEM、FT-IR、TG等手段对所制备样品进行了表征,结果表明:75℃条件下,通氨时间为1 h,产品粒度分散均匀,二次粒径为0.69μm;产品形貌为六方片状;其(001)面与(101)面特征衍射峰的强度比值I001/I101为0.71;在322～396℃的分解失重为24.9%,最高吸热温度为376.2℃,技术指标符合氢氧化镁阻燃剂的使用要求;对罗丹明b溶液的光降解率为56.3%。     

Preparation and characterization of Y3Al5O12:Ln (Ln=Eu,Ce) phosphor powders by ultrasonic atomization and co-precipitation process

A novel technique for YAG:Ln (Ln=Eu, Ce) phosphor powder synthesis with a nanocrystalline structure was developed. Nanocrystalline YAG:Ln powder was prepared by an ultrasonic atomization and co-precipitation method using a mixture solution of ammonium hydroxide(NH₃·H₂O) and ammonium hydrogen carbonate(NH₄HCO₃) as precipitant. The as-prepared nano-powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and fluorescence spectrometer. The obtained phosphor powders were homogenous and in size of 50-70 nm. The results demonstrated that by using ultrasonic atomization and co-precipitation process, we could synthesize a good quality YAG:Ln (Ln=Eu, Ce) phosphor powder that had many potential applications.     

Effect of Molybdenum Additions on Compaction during Sintering of Fine-Grained Iron-Copper Pseudoalloys

The effect of added molybdenum powder on compaction and the properties of sintered fine-grained iron-copper pseudoalloys is studied. The original powder mixtures are prepared by mechanical alloying, and the original powder particle size in mixtures does not exceed 0.5 μm. Specimens are sintered in the range 600-1130°C. It is shown that addition of molybdenum powder to the original charge accelerates compaction of fine pseudoalloys in both the solid phase and liquid-phase sintering compared with compaction of the same pseudoalloys without adding molybdenum. After solid-phase sintering the maximum relative density of specimens is 98.8%, and after liquid-phase sintering it is 99.3%. The main reasons for acceleration of compaction are prolonged retention of a fine-grained structure of sintered specimens up to the melting temperature for the phase based on copper and mutual diffusion between iron and molybdenum; to a significant extent the latter occurs during specimen heating in the solid phase.     

MAX phase foams produced via powder metallurgy process using water soluble space holder

Abstract

There have been few systematic studies of the fabrication and properties of porous MAX phase microstructures despite the potential applications of these materials. A simple, low cost, eco-friendly PM method has been developed to prepare MAX phase foams from commercial Ti₂AlC powder, using crystalline carbohydrate as space holder. This method involves: mixing Ti₂AlC powder with crystalline carbohydrate, pressing to form a green body, removal of the space holder and sintering. Compaction was achieved by uniaxial pressing (UP) and cold isostatic pressing (CIP). Control of porosity was achieved by varying the particle size (three ranges between 250 and 1000?μm), and volume fractions (20, 40 and 60%) of space holder. The foams were characterised and the porosity compared with the expected values. Optimal conditions for this novel processing technique were established with the aim of controlling the final microstructures and properties of the Ti₂AlC foams.