Method for preparing cobalt powder from cobalt oxalate

A technology of cobalt oxalate and cobalt powder, which is applied in the field of cobalt oxalate hydrogen reduction to prepare cobalt powder, which can solve the problems of complex preparation process, undisclosed, and difficult control of the final product phase composition ratio, and achieve simple process and crystal form Proportional Control for Precise Effects

Active Publication Date: 2022-05-06
安徽寒锐新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to meet the needs of ball milling without affecting the properties of the alloy, it is particularly important to control the relative content of the crystal form in the preparation of cobalt powder. However, there are only qualitative studies in the current method, and it is difficult to control the phase composition ratio of the final product. within a small range
[0003] The patent application number is CN101653830B, which discloses a method for hydrogen

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Introduce argon gas into the furnace for 30 minutes, detect that the oxygen content in the tail gas is less than 0.1%, slowly raise the temperature to 120°C for dehydration, and the heating rate is 5°C / min.

[0027] Switch to feeding hydrogen into the furnace to continue heating, the hydrogen flow rate is 1.5 L / min, the heating rate is 5°C / min, the temperature is raised to the set reduction temperature of 350°C, and the reduction is carried out at 350°C for 165 minutes.

[0028] After the reaction, the product is cooled with the furnace, the cooling rate is less than 3°C / min, after cooling to room temperature, the hydrogen gas is turned off and the product is taken out and sealed in vacuum.

[0029] The obtained cobalt powder has a Fisherman's particle size of 0.9 μm, and the results of XRD detection and quantitative calculation are: HCP content 47.4%, FCC content 52.6%.

Embodiment 2

[0031] Introduce argon gas into the furnace for 30 minutes, detect that the oxygen content in the tail gas is less than 0.1%, slowly raise the temperature to 120°C for dehydration, and the heating rate is 5°C / min.

[0032] Switch to feeding hydrogen into the furnace to continue heating, the hydrogen flow rate is 1.5 L / min, the heating rate is 5°C / min, the temperature is raised to the set reduction temperature of 400°C, and the reduction is carried out at 400°C for 165 minutes.

[0033] After the reaction, the product is cooled with the furnace, the cooling rate is less than 3°C / min, after cooling to room temperature, the hydrogen gas is turned off and the product is taken out and sealed in vacuum.

[0034] The resulting cobalt powder has a Fisherman's particle size of 0.96 μm. XRD detection and quantitative calculation results show that the HCP content is 18.9%, and the FCC content is 81.1%.

Embodiment 3

[0036] Introduce argon gas into the furnace for 30 minutes, detect that the oxygen content in the tail gas is less than 0.1%, and slowly raise the temperature to 120°C with a heating rate of 5°C / min.

[0037] Switch to feeding hydrogen into the furnace to continue heating, the hydrogen flow rate is 1.5 L / min, the heating rate is 5°C / min, the temperature is raised to the set reduction temperature of 480°C, and the reduction is carried out at 480°C for 165 minutes.

[0038] After the reaction, the product is cooled with the furnace, the cooling rate is less than 3°C / min, after cooling to room temperature, the hydrogen gas is turned off and the product is taken out and sealed in vacuum.

[0039] The obtained cobalt powder has a Fisherman's particle size of 1.95 μm. XRD detection and quantitative calculation show that the HCP content is 5.2%, and the FCC content is 94.8%.

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PUM

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Abstract

The invention provides a method for preparing cobalt powder from cobalt oxalate. The method comprises the following steps that firstly, the cobalt oxalate powder is heated to the reduction temperature under the condition that hydrogen is introduced; and secondly, the cobalt oxalate powder and hydrogen react at the reduction temperature to prepare cobalt powder, and then the cobalt powder is cooled to the normal temperature. The reduction temperature corresponds to the crystal form content in the cobalt powder, and the crystal form of the cobalt powder is controlled within a certain proportion range by controlling the reduction temperature. The preparation method provided by the invention has the advantages of simple process and relatively accurate crystal form proportion control.

Description

technical field [0001] The invention relates to the field of preparing cobalt powder by hydrogen reduction, in particular to a method for preparing cobalt powder by hydrogen reduction of cobalt oxalate. Background technique [0002] Because of its unique chemical properties, cobalt is often used as an important constituent phase in cemented carbide, diamond tools and magnetic materials. Cobalt is an allotropic polymorphic metal, which can undergo crystal transformation under certain conditions. Studies have shown that cobalt has two stable crystal forms: the face-centered cubic structure (FCC) which is stable at high temperature, and the hexagonal close-packed structure (HCP) which is stable at room temperature. Face-centered cubic cobalt has 12 slip systems and has better plasticity, which can make cemented carbide show better toughness in response to external impact. Close-packed hexagonal cobalt has only three slip systems, showing more brittleness, which is conducive t...

Claims

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Application Information

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IPC IPC(8): B22F9/22
CPCB22F9/22
Inventor 余杰王朝安杨生泉梁闯
Owner 安徽寒锐新材料有限公司
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