Preparation method of low-oxygen-content high-dispersion nanometer spherical cobalt powder

A low-oxygen content, high-dispersion technology, applied in nanotechnology and other directions, can solve the problems of poor dispersibility and fluidity, large particle size, and high powder oxygen content, and achieve improved dispersibility and fluidity, narrow particle size distribution, and dispersibility. Good results

Active Publication Date: 2021-05-28
GRIMAT ENG INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the liquid phase precipitation-hydrogen reduction method, the cobalt powder produced by the oxalate precipitation-hydrogen reduction method has low purity and large particle size, about 1.0-3.0 μm, dendritic shape and uneven particle size distribution, which cannot meet the ultra-fine / Nano WC-Co cemented carbide requirements
A large number of research results show that using (NH4)2CO3 instead of oxalic acid as the precipitation of Co2+ It can obtain nearly spherical Co powder with a particle size of less than 100nm, an oxygen content of less than 0.8wt%, and a close-packed hexagonal phase structure, but there are problems such as high oxygen content of the powder, poor dispersibility and fluidity.

Method used

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  • Preparation method of low-oxygen-content high-dispersion nanometer spherical cobalt powder

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preparation example Construction

[0027] Specifically, the preparation method of the low-oxygen-content high-dispersion nano-spherical cobalt powder of the present invention comprises the following steps:

[0028] (S1) will analyze pure cobalt salt, (NH 4 ) 2 CO 3 respectively dissolved in deionized water to form a cobalt salt solution, (NH 4 ) 2 CO 3 Solution, the phenolic resin is dissolved in ethanol and is made into phenolic resin ethanol solution;

[0029] Cobalt salt solution is CoCl in the step (S1) 2 、CoSO 4 , Co(NO 3 ) 2 One or more of them, the concentration of cobalt salt solution is 1~1.1mol / L; (NH 4 ) 2 CO 3 The concentration of the solution is 1.2-1.3 mol / L. The mass concentration of the phenolic resin in the phenolic resin ethanol solution is 3-4 wt%.

[0030] (S2) After mixing the cobalt salt solution and the phenolic resin ethanol solution obtained in step (S1), add (NH 4 ) 2 CO 3 The solution undergoes a precipitation reaction, and the precipitate is separated after the reacti...

Embodiment 1

[0037] Preparation of spherical cobalt powder with oxygen content less than 0.4wt%, high dispersion and particle size less than 100nm:

[0038] (1) The analytically pure cobalt salt CoCl 2 ·6H 2 O, precipitant (NH 4 ) 2 CO 3 respectively dissolved in deionized water to form a solution, in which CoCl 2 The concentration of the solution is 1.1mol / L, (NH 4 ) 2 CO 3 The concentration of the solution is 1.3mol / L, and at the same time, the phenolic resin is dissolved in absolute ethanol to prepare a phenolic resin ethanol solution with a mass concentration of 4wt%.

[0039] (2) Take 100ml of CoCl 2 Solution (quality is 114.3 grams) is placed in reactor, then reactor is placed in 50-60 ℃ of water baths, adds step (1) gained mass concentration in reactor and is 1.26 grams of phenolic resin ethanol solution of 4wt% (for CoCl 2 1.1wt% of the solution quality), fully mix in the reaction kettle, then add 105ml of (NH 4 ) 2 CO 3 solution (the Co in the solution at this time 2...

Embodiment 2

[0042] Preparation of spherical cobalt powder with oxygen content of 0.5-0.6wt%, high dispersion and particle size less than 100nm:

[0043] (1) The analytically pure cobalt salt CoCl 2 ·6H 2 O, precipitant (NH 4 ) 2 CO 3 respectively dissolved in deionized water to form a solution, in which CoCl 2 The concentration of the solution is 1mol / L, (NH 4 ) 2 CO 3 The concentration of the solution is 1.2mol / L, and at the same time, the phenolic resin is dissolved in absolute ethanol to prepare a solution with a mass concentration of 4wt%.

[0044] (2) Take 100ml of CoCl 2 Solution (mass is 113.0 grams) is placed in reactor, then reactor is placed in 50-60 ℃ of water baths, in reactor, add mass concentration and be that phenolic resin ethanol solution 1.02 grams of 4wt% (as CoCl 2 0.9wt% of the solution quality), fully mix in the reactor, then add 100ml of (NH 4 ) 2 CO 3 solution (the Co in the solution at this time 2 + :CO 3 2- Molar ratio 1:1.2) carries out precipita...

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Abstract

The invention discloses a preparation method of low-oxygen-content high-dispersion nanometer spherical cobalt powder, and belongs to the technical field of metal materials. The method comprises the following step that hydrogen serves as a reducing agent to reduce a Co-containing precursor to prepare the nanometer spherical cobalt powder, and the Co-containing precursor is doped with phenolic resin. The particle size of the cobalt powder prepared through the preparation method is less than or equal to 100 nm, the cobalt powder is spherical, particle size distribution is narrow, dispersity is good, the oxygen content is less than 0.6 wt%, and compared with existing cobalt powder preparation technology, the preparation method has the remarkable technical advantages.

Description

technical field [0001] The invention belongs to the technical field of metal material preparation, and in particular relates to a preparation method of low-oxygen content and highly dispersed nano-spherical cobalt powder. Background technique [0002] In the sintering process of ultrafine / nano WC-Co cemented carbide, the binder phase Co plays a crucial role in both densification and microstructural evolution, in order to avoid ultrafine / nano WC-Co hard In the early stage of the alloy, the sintered crystal grains grow, and ultrafine / nano Co powder is usually used as the initial raw material. The particle size, sphericity, dispersion and fluidity of the initial Co powder have a great influence on the cobalt phase distribution and alloy properties in ultrafine and nanocrystalline WC-Co alloys. [0003] The ideal Co powder for the preparation of ultrafine / nano WC-Co cemented carbide should have ultrafine particle size (less than 1 μm), good sphericity, high dispersion and high ...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): B22F9/22B82Y40/00
CPCB22F9/22B82Y40/00
Inventor李艳周增林何学良惠志林谢元锋陈文帅何云龙李雄潘贤斌谢臣珍兰秋平
OwnerGRIMAT ENG INST CO LTD