Spherical rhenium powder preparation method

A rhenium powder and spherical technology, applied in the field of spherical rhenium powder preparation, can solve the problems of low adsorption performance of small particle powder, small particle size of spherical powder, difficult application in 3D printing field, etc., and achieves reduction of fine powder loss and good powder densification performance. , the effect of low content of hollow spheres

Active Publication Date: 2018-03-27
CHONGQING MATERIALS RES INST
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  • Abstract
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Problems solved by technology

[0003] The method for preparing spherical rhenium powder has following several kinds at present: 1. first prepare ammonium rhenate powder particle with spray milling method, carry out reduction to obtain rhenium powder, then carry out the process of plasma spheroidization, but the rhenium powder particle size that this process makes is small , the particles are usually below 10 μm, and the particle size of the spherical powder after spheroidization is small, which is difficult to apply in the field of 3D printing; 2. The rhenium powder is prepared by reducing large particles of ammonium rhenate, and the irregular rhenium powder particles are subjected to plasma ball after grinding Chemical production of spherical rhenium powder, this method has many defects such as hollows and pores in the large particles of spherical rhenium powder, which seriously affects the compactness of the powder.
The disadvantage of the above method is that due to the large number of voids in the rhenium powder raw material particles, in the plasma spheroidization process, the rhenium powder particle raw material enters the high-temperature plasma torch area from the powder feeder, and the metal particles absorb heat and melt under the action of the surface tension of the metal liquid. form a sphere
The time for rhenium powder particles to pass through the high-temperature plasma area is only tens of milliseconds, and the heat absorbed by rhenium powder can only melt rhenium powder particles below 10 microns, which is not enough to completely melt the inside of large rhenium powder particles to eliminate internal gas or fill internal voids After the surface layer of the particles is melted, a small amount of metal liquid is formed to cover the particles to form a spherical shape under the action of surface tension. After cooling, spherical rhenium powder is obtained, but the voids and pores still exist.
The current plasma spheroidization equipment is usually equipped with a multi-stage powder collection system. The cooling gas flows from the first-stage powder collection tank to the last-stage powder collection tank. Setting the cooling gas flow rate according to the particle size (D50) of most powders will inevitably lead to The small-particle powder is too stressed to deposit in the first-stage collection tank, but is carried by the carrier gas to the second-stage or third-stage powder collection tank or pipeline. The small-particle powder has strong adsorption performance and small amount, and usually adheres to the In the inner wall of the pipeline, it cannot be effectively recovered, resulting in a low yield of spherical powder

Method used

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Examples

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Embodiment 1

[0027] Example 1 Preparation of spherical rhenium powder with particle size ranging from 0 to 45 μm

[0028] Weigh 1.5kg of high-purity ammonium rhenate raw material, roast ammonium rhenate at 280°C for 1h, the roasting atmosphere is hydrogen, and the flow rate is controlled at 3L / min;

[0029] After cooling, crush, grind, and pass through a 500-mesh sieve to obtain rhenium oxide powder with a particle size of less than 25 μm;

[0030] For mixing, put rhenium oxide powder, 500ml of alcohol, and 150g of ammonium rhenate into a vacuum mixing tank, vacuumize to -0.08Mpa, mix for 4 hours, and pump air every 2 hours to discharge the gas in the rhenium oxide particles. Let the ammonium rhenate solution enter the pores for filling;

[0031] After taking it out, heat and dry it in a water bath, crush it, and put it into a molybdenum boat;

[0032] Put it into a molybdenum wire furnace with hydrogen atmosphere at room temperature for two-stage reduction, 280°C for 1h in hydrogen atmo...

Embodiment 2

[0043] Example 2 Preparation of spherical rhenium powder with particle size ranging from 75 to 100 μm

[0044] Weigh 1.5kg of high-purity ammonium rhenate raw material, roast ammonium rhenate at 280°C for 1h, the roasting atmosphere is hydrogen, and the flow rate is controlled at 3L / min.

[0045] After cooling, crush, grind, and pass through a 200-mesh sieve to obtain rhenium oxide powder with a particle size of less than 74 μm.

[0046] For mixing, put rhenium oxide powder, 500ml of alcohol, and 150g of ammonium rhenate into a vacuum mixing tank, vacuumize to -0.08Mpa, mix for 4 hours, and pump air every 2 hours.

[0047] After taking it out, heat and dry it in a water bath and crush it.

[0048] Put it into a molybdenum wire furnace with hydrogen atmosphere at room temperature for two-stage reduction, 280°C for 1 hour (flow rate 4L / min), and 900°C for 2 hours, both in hydrogen atmosphere (flow rate 8L / min).

[0049] After taking out, crush, grind, and pass through a 180-mesh...

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Abstract

The invention relates to a spherical rhenium powder preparation method. The spherical rhenium powder preparation method is used for preparing spherical rhenium powder with the particle size ranging from 10 microns to 100 microns. According to the spherical rhenium powder prepared through the method, a small number of holes are formed inside a powder body, the content of hollow spheres is low, theapparent density is high, and powder compactness is good. According to the method, the plasma spherizing process is optimized, losses of the minute powder are reduced, and the yield of the spherical rhenium powder is increased.

Description

technical field [0001] The invention relates to a method for preparing a material, in particular to a method for preparing spherical rhenium powder. Background technique [0002] Spherical rhenium powder has the characteristics of good fluidity, bulk density, and high tap density, and is widely used in the fields of 3D printing, hot pressing, and plasma spraying. Among them, large-particle spherical rhenium powder is mostly used in the fields of 3D printing and plasma spraying. [0003] The method for preparing spherical rhenium powder has following several kinds at present: 1. first prepare ammonium rhenate powder particle with spray milling method, carry out reduction to obtain rhenium powder, then carry out the process of plasma spheroidization, but the rhenium powder particle size that this process makes is small , the particles are usually below 10 μm, and the particle size of the spherical powder after spheroidization is small, which is difficult to apply in the field...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/22B22F9/04B22F1/00
CPCB22F9/04B22F9/22B22F2999/00B22F2998/10B22F1/065B22F1/14B22F2202/13
Inventor 王小宇刘奇蒋春东薄新维唐鸿滨王焱辉陈德茂刘成超
Owner CHONGQING MATERIALS RES INST
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