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Low-oxygen content submicron cobalt powder and cobalt oxalate precursor and manufacturing method thereof

A technology of micron cobalt powder and manufacturing method, which is applied in the field of metallurgy and chemical industry, can solve problems such as difficult stable operation, easy fire, poor stability, etc., and achieve the effect of easy and stable control of the reaction process

Active Publication Date: 2013-03-27
GEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] It can be seen from the above table that the Fischer particle size and oxygen content of cobalt powder products produced by domestic enterprises are difficult to be controlled in a low range at the same time; traditional submicron cobalt powder tends to contain oxygen in finer submicron products. Increase, the finer sub-micron powder is very easy to catch fire in the reduction process, resulting in poor stability of the process. Although the process steps are simple, it is difficult to run stably in the whole production process, the preparation is difficult, and the production efficiency and product quality are relatively low. Low; in a word, to achieve stable production of high-quality submicron cobalt powder (especially 0.5-0.8μm cobalt powder), no matter using cobalt carbonate precursor or cobalt oxalate precursor, the existing synthesis process or reduction Processes have encountered severe challenges

Method used

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  • Low-oxygen content submicron cobalt powder and cobalt oxalate precursor and manufacturing method thereof
  • Low-oxygen content submicron cobalt powder and cobalt oxalate precursor and manufacturing method thereof
  • Low-oxygen content submicron cobalt powder and cobalt oxalate precursor and manufacturing method thereof

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Experimental program
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Effect test

Embodiment 1

[0040] Implement CoCO 3 Wet slurry, solid-liquid ratio 1:2; oxalic acid solution with a concentration of 0.8mol / L, molar ratio n CoCO 3 : N H 2 C 2 O 4 =1∶2 ready to mix, preheat the solution to 25°C before the reaction, and reduce H within 15 minutes 2 C 2 O 4 CoCO solution added 3 In the slurry, react with constant temperature stirring for 3 hours. Separate the precipitate from the solution, filter and wash with clean water, dry at 100-150°C for 15-18 hours, grind and crush the dry powder and pass it through a 100-mesh sieve to detect the obtained cobalt oxalate precursor The cobalt content is 32.96%wt, and the loose density is 0.19g / cm 3 , D 50 The cobalt oxalate precursor is reduced at 300-350°C to obtain cobalt powder. The Fischer particle size of the unbroken cobalt powder is 0.86 μm and the oxygen content is 0.52%wt. The whole process is stable and not easy to catch fire.

Embodiment 2

[0042] Implement CoCO 3 Wet slurry, solid-liquid ratio 1:4; preparation of oxalic acid solution with a concentration of 0.8mol / L, molar ratio n CoCO 3 : N H 2 C 2 O 4 =1:1.3 is ready to be mixed, the solution is preheated to 25 ℃ before the reaction, and the H 2 C 2 O 4 CoCO solution added 3 In the slurry, react with constant temperature stirring for 3 hours. Separate the precipitate from the solution, filter and wash with clean water, dry at 80-120°C for 15-18 hours, grind and crush the dry powder and pass it through a 100-mesh sieve to detect the obtained cobalt oxalate precursor The cobalt content is 32.79%wt, and the loose density is 0.14g / cm 3 , D 50 The cobalt oxalate precursor is reduced at 300-350°C to obtain cobalt powder. The Fischer particle size of the unbroken cobalt powder is 0.60 μm and the oxygen content is 0.43%wt. The whole process is stable and not easy to catch fire.

Embodiment 3

[0044] Implement CoCO 3 Wet slurry, solid-liquid ratio 1:4; preparation of oxalic acid solution with a concentration of 0.8mol / L, molar ratio n CoCO 3 : N H 2 C 2 O 4 =1:1.3 is ready to mix, preheat the solution to 25°C before the reaction, and remove H within 40min 2 C 2 O 4 CoCO solution added 3 In the slurry, react with constant temperature stirring for 3 hours, separate the precipitate from the solution, filter and wash with clean water, dry at 100-150°C for 15-18 hours, grind and crush the dry powder and pass it through a 100-mesh sieve to detect the obtained cobalt oxalate precursor The content of cobalt is 32.67%wt, and the bulk density is 0.22g / cm 3 , D 50 The cobalt oxalate precursor is reduced at 300-350°C to obtain cobalt powder. The Fischer particle size of the unbroken cobalt powder is 0.55 μm and the oxygen content is 0.61%wt. The whole process is stable and not easy to catch fire.

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Abstract

The invention relates to low-oxygen content submicron cobalt powder and a cobalt oxalate precursor and a manufacturing method thereof, wherein the low-oxygen content submicron cobalt powder is prepared by the steps of preparing the cobalt oxalate precursor through the solid-liquid reaction of cobalt carbonate powder and an oxalate solution and then reducing the cobalt oxalate precursor. The low-oxygen content submicron cobalt powder can keep low oxygen content in fine submicron-level products, is difficult to fire in the reduction procedure, is easy to stably run in all processes of the production process and has convenient preparation.

Description

technical field [0001] The invention relates to the field of metallurgy and chemical industry, more specifically, the invention relates to a metal powder and a manufacturing method thereof. Background technique [0002] Cobalt powder is widely used in the field of metallurgy and chemical industry, and is an important raw material for the production of metallurgical and chemical products such as battery electrodes, high hardness alloys, diamond tools, and catalyst carriers. [0003] With the advancement of technology, the market's requirements for the quality of cobalt powder have become harsh and diverse. In addition to the requirements for particle morphology, customers are increasingly asking for indicators such as particle size, oxygen content, and bulk density of cobalt powder. Special and special requirements; Among them, cobalt powder with a particle size ranging from 100nm to 1μm is called by the industry: submicron cobalt powder, and low-oxygen submicron cobalt powde...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24
Inventor 许开华何显达韩红涛
Owner GEM CO LTD
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