Characterization of nanometer tungsten powders

Three types of tungsten powders were prepared by hydrogen reduction of three precursor powders at low temperature, which were used as samples, and were then characterized by Brunauer-Emmer-Teller （BET） method, scanning electron microscopy （SEM）, transmission electronic microscopy （TEM）, small angle X-ray scattering （SAXS）, and field-emission scanning election microscopy （FESEM） respectively. The results showed that although BET and SEM could not characterize the particle size of nanometer powders, they were important means of assistance to exclude non-nanometer powders. TEM and FESEM could directly measure the particle size of nanometer powders, but this needs a lot of time, to count the average particle size and particle size distribution. SAXS could not describe the state of agglomeration. By the combination of FESEM and SAXS, the particle size, particle size distribution, and particle shape of nanometer powders could be precisely characterized.

Effect of rare earth element cerium on preparation of tungsten powders

Tungsten powders and Ce doped powders were prepared by hydrogen reduction combined with the liquid-solid doping method. The phase composition, particle size and powder morphology of Ce doped tungsten powders were analyzed by X-ray diffrac-tion, scanning electron microscopy and transmission electron microscopy, respectively. The results indicated that 10000 ppm Ce doped tungsten oxide powders were consisted of WO3 phase and Ce4W9O33 phase. The hydrogen reduction of Ce doped tungsten powders was basically accomplished at 800 oC for 3 h. The size of Ce doped W powders was remarkably decreased compared to the undoped W powders. The phase of Ce4W9O33 was reduced to Ce2 （WO4）3 phase and Ce2W2O9 phase during the process of hydrogen reduction. Moreover, Ce2 （WO4）3 phase and Ce2W2O9 phase were observed form their morphologies, where the doping content of Ce was more than 100 ppm. The ternary phase embedding into W particles was assigned to Ce2 （WO4）3, while the ternary phase distrib-uting among W particles corresponded to Ce2W2O9. The phase of Ce2 （WO4）3 might be the nucleus of W particles and increase the number of the nucleus. And the particles of Ce2W2O9 covered WO2 particles and might inhibit the growth of W particles. These two reasons resulted in the decrease of the size of Ce doped W particles. Uniform fine W powders were fabricated with the doping content of Ce more than 100 ppm.

Hot-pressed sintering of W/Cu functionally graded materials prepared from copper-coated tungsten powders

The three-layered(W-60 vol%Cu/W-40 vol%Cu/W-20 vol%Cu)W/Cu functionally graded material(FGM)containing a Cu network structure was fabricated at different temperatures by hot-pressed sintering produced from copper-coated tungsten powders.The effects of various sintering temperatures on relative density,microstructure,thermal conductivity,hardness and flexural strength were investigated.Scanning electron microscopy(SEM)and X-ray diffraction(XRD)analysis show that a Cu network extends throughout the W/Cu FGM specimens sintered at 1065℃and the graded structure can be retained perfectly,and W particles are distributed homogeneously.The low-temperature sintering densification of W/Cu FGM arises because the sintering mode of the copper-coated tungsten particles includes just sintering Cu to Cu,rather than Cu to W,Cu to Cu and W to W,as required for conventional powder particles.The relative density of W/Cu FGM sintered at 1065℃for 3 h under a load of25 MPa is 96.1%.The thermal conductivity is up to204 W·m^-1·K^-1 at normal temperature and 150 W·m^-1·K^-1at 800℃.And the Vickers hardness varies with the gradient of different layers from 3.34 to 4.05 GPa.

A Study of Scandia Doped Tungsten Nano-Powders

Scandia and rhenium doped tungsten powders were prepared by solid-liquid doping combined with two-step reduction method. The particle size of doped tungsten and distribution of scandia and rhenium were studied by SEM, EDS, XRD and granularity analysis. Experimental results showed that scandia distributed evenly on the surface of tungsten particles. Addition of scandia and rhenium decreased the particle size of doped tungsten, and the more the content of scandia and rhenium, the smaller the doped tungsten particles. Tungsten powders doped with 3 % Sc2O3 and 3 % Re （mass fraction） had an average size of about 80 nm in diameter. The mechanism of the decrease in the tungsten particle size was discussed.

Study on the RF inductively coupled plasma spheroidization of refractory W and W-Ta alloy powders

Spherical powders with good flowability and high stacking density are mandatory for powder bed additive manufacturing. Nevertheless, the preparation of spherical refractory tungsten and tungsten alloy powders is a formidable task. In this paper, spherical refractory metal powders processed by high-energy stir ball milling and RF inductively coupled plasma were investigated. By utilizing the technical route, pure spherical tungsten powders were prepared successfully, the flowability increased from 10.7 s/50 g to 5.5 s/50 g and apparent density increased from 6.916 g cm-3 to 11.041 g cm-3. Alloying element tantalum can reduce the tendency to micro- crack during tungsten laser melting and rapid solidification process. Spherical W-6Ta （%wt） powders were prepared in this way, homogeneous dispersion of tantalum in a tungsten matrix occurred but a small amount of flake-like shape particles appeared after high-energy stir ball milling. The flake-like shape particles can hardly be spheroidized in subsequent RF inductively coupled plasma process, might result from the unique suspended state of flaky particles under complex electric and magnetic fields as well as plasma-particle heat exchange was different under various turbulence models. As a result, the flake-like shape particles cannot pass through the high-temperature area of thermal plasma torch and cannot be spheroidized properly.

Preparation of Ultrafine Tungsten Powder by Sol-Gel Method

Sol-gel method was employed for the preparation of nanoscale tungsten powder. The effects of different preparation conditions on particle size were discussed and the optimum preparation condition was found. The products were characterized by X-ray diffraction, scan electron microscopy and so on. The results show that the intermediate is monoclinic WO3, its particle shape is approximately spherical, and the particle size distribution is narrow. The average particle size is about 60 nm. After deoxidization, WO3 turns into cubic tungsten powder with small particle size （average particle size about 120 nm） and narrow size distribution.

STUDY OF PREPARATION PROCESS OF TUNGSTEN POWDER BY SHS WITH A MAGNESIUM THERMIT STAGE

Tungsten powder was fabricated from the system CaWO4-Mg by self-propagating high-temperature synthesis (SHS) with a magnesium thermit stage. The physic-chemical change during heating and the effects of pressure of sample and diluents (W powder) on product have been studied. The experimental results show that the porosity of combustion product and the particle size of final tungsten powder decrease with increasing pressure of sample. Addition of diluents could increase the particle size of final tungsten powder. The purity of tungsten is improved by leaching in NaOH solution. The results of spectral analysis and particle size distribution of final tungsten powder show that the final Tungsten powder has a median diameter of 0.87μm,specific surface area of 1.09m2/g and purity of above 99.0%.

Effect of Y_(2)O_(3)doping on preparation ultrafine/nano-tungsten powder and refinement mechanism

In this study,ultrafine/nano W-Y_(2)O_(3)composite powders were synthesized by spray drying,roasting and two-step hydrogen reduction using ammonium metatungstate and yttrium nitrate as raw materials.The mechanism of the influence of Y_(2)O_(3)on the growth of WO_(2.72)and the particle refinement of tungsten powder is discussed.The effect of Y_(2)O_(3)particles on the reduction behavior of tungsten powder was investigated using scanning electron microscopy to study the near surface morphology and X-ray diffraction for phase ID(composition)and crystal structural changes for the reduced powders at each step.The results show that the doping of 0.3 wt.%Y_(2)O_(3)can significantly increase the aspect ratio of WO_(2.72)in the first step of hydrogen reduction.Moreover,Y_(2)O_(3)can effectively inhibit the growth of tungsten particles in the hydrogen reduction process.Therefore,The Y_(2)O_(3)-doped tungsten powders have finer particles and a narrower particle size distribution range than the undoped powders.The average particle diameter of 0.3 wt.%Y_(2)O_(3)doping tungsten powder was in the range of 90-120 nm.

Spherical modification of tungsten oxide powder and its mechanism analysis

Owing to its high production costs, complexity of equipment, and difficulty in controlling parameters, spherical or subglobose tungsten powder preparation method cannot meet the demand of industrial production. Tungstic oxide powder was treated by particle composite system and its effects were studied. Morphologies of par- ticles were investigated by scanning electron microscopy （SEM）. Particle size analysis was carried out and the related mechanism was discussed. The results show that the processing effect is best when the rotational speed is set at 4,000 r.min-1 for 15 rain： the powder particles become nearly spherical and their sharp edge angles are rounded off and reshaped. When the processing time is 60 min, the powders smash to pieces because of too much energy inputting. So the test results, such as grain size distribution, can be explained well. Nearly spherical tungsten powder is obtained after reduction at 780 ℃ for 2 h and its flow ability is significantly improved.

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 diffrac-tion 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 pre-cursor 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 scan-dium were obtained.

Spherical modification of tungsten powder by particle composite system

Owing to contradiction between increasing demand of spherical tungsten powder and limitation of traditional manufacturing technology,a novel preparation method was developed to sphericize the polygonal tungsten powder by means of modification of particle composite system.Tungsten powder particles were modified by par-ticle composite system,and detailed characterization by scanning electron microscopy(SEM)was studied.Particle size distribution and function mechanism were analyzed,and the internal relationship between average diameter and processing time was discussed.The results show that the spherical tungsten powder with an average diameter of 6.41μm is obtained from polyhedral tungsten powder with an average diameter of 7.50μm.The spherical effect could be achieved(sharp edge angles of particles are rounded off and reshaped)when the processing time is over 30 min.The relationship between average diameter(d)and pro-cessing time can be described by the exponential decay model,which provides a good interpretation for the process of modification.The relationship between them can be expressed by the equation d=1.87406exp(-x/8.92718)+6.4182.The proposed method could readily enable large-scale production of spherical tungsten powder.