CN106799499A - A kind of preparation method of spherical cobalt powder - Google Patents
A kind of preparation method of spherical cobalt powder Download PDFInfo
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- CN106799499A CN106799499A CN201611072780.6A CN201611072780A CN106799499A CN 106799499 A CN106799499 A CN 106799499A CN 201611072780 A CN201611072780 A CN 201611072780A CN 106799499 A CN106799499 A CN 106799499A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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Abstract
The invention discloses a kind of preparation method of spherical cobalt powder, following steps are specifically included：Step 1, adds reactor to be reacted cobalt salt and ammonium bicarbonate solution cocurrent, controls course of reaction pH value so that system pH is adjusted to 7.0 ± 0.1 after half an hour；Step 2, continues cocurrent and adds cobalt salt and ammonium bicarbonate solution, keeps the pH value of step 1 constant, continues to react and precipitates；Step 3, the solution after being precipitated to step 2 carries out separation of solid and liquid and drying, obtains spherical cobaltous carbonate；Step 4, the cobalt carbonate of step 3 is reduced in hydrogen atmosphere；Step 5, the cobalt carbonate after step 4 is reduced is cooled down, that is, obtain spherical cobalt powder.The cobalt powder of this method production is the second particle that primary particle is reunited, and can be sufficiently mixed with tungsten carbide, the efficiency and quality of mixing is improved, while increased the intensity of hard alloy.
Description
Technical field
The invention belongs to metal powder material fabricating technology field, and in particular to a kind of preparation side of spherical cobalt powder
Method.
Background technology
Existing cobalt powder is that the cobalt carbonate high-temperature hydrogen reduction of random reunion is formed, and is then crushed again, and what is obtained divides
The cobalt powder particle that a bad single dispersing of property or part are reunited is dissipated, this conventional cobalt powder current AD and BET is both less than 1g/cm3
And 1m2/ g, this means that the actual particle of cobalt powder than larger, and structure is fluffy between particle and particle, can so cause hard
WC and cobalt powder batch mixing during matter alloy use is not uniform enough, and alloy dimensional discrepancy is excessive etc..
The content of the invention
It is an object of the invention to provide a kind of preparation method of spherical cobalt powder, secondary reunited by primary particle
Grain, bulk density is big, and mobility is more preferable.
The technical solution adopted in the present invention is that a kind of preparation method of spherical cobalt powder specifically includes following steps：
Step 1, adds reactor to be reacted cobalt salt and ammonium bicarbonate solution cocurrent, controls course of reaction pH value so that half
System pH is adjusted to 7.0 ± 0.1 after hour；
Step 2, continues cocurrent and adds cobalt salt and ammonium bicarbonate solution, keeps the pH value of step 1 constant, continues to react and precipitates；
Step 3, the solution after being precipitated to step 2 carries out separation of solid and liquid and drying, obtains spherical cobaltous carbonate；
Step 4, the cobalt carbonate of step 3 is reduced in hydrogen atmosphere；
Step 5, the cobalt carbonate after step 4 is reduced is cooled down, that is, obtain spherical cobalt powder.
The features of the present invention is also resided in,
Cobalt salt in step 1 is the one kind in cobalt chloride, cobaltous sulfate, cobalt acetate.
The concentration of cobalt salt is 80-140g/l in the step 1, and flow is 1-2.5L/h.
PH value in the step 1 is adjusted according to the flow of carbon ammonium.
The concentration of carbon ammonium is 220g/l in the step 1.
The temperature reacted in the step 2 is 40 DEG C, and the time of reaction is 1-5h.
Stir speed (S.S.) in the step 2 is 80-220r/min.
Reduction in the step 4 is carried out in push rod furnace, and the temperature of reduction is 280-430 DEG C, and the time of reduction is 3-
8h。
The flow of hydrogen is 400-1000L/h in the step 4.
The time cooled down in the step 5 is 4-8h.
The beneficial effects of the invention are as follows, a kind of preparation method of spherical cobalt powder of the invention, the cobalt powder of this technique productions is very
The second particle that thin primary particle is reunited, the size of these primary particles is averagely micro- 0.7 between 0.2-2 microns
Rice or so, the size of second particle is between 3-6 microns, and AD and BET are bigger than conventional cobalt powder, so make in hard alloy
With process, primary particle can and carbide together ball milling and scatter, a cobalt of such practical function and tungsten carbide surface
The size of particle is actually Nano grade, so can be sufficiently mixed with WC, improves the efficiency and quality of mixing, while increasing
The intensity of hard alloy.
Brief description of the drawings
Fig. 1 provides the electron microscope of the cobalt powder prepared in embodiment 1 for the present invention；
Fig. 2 provides the electron microscope of the cobalt powder prepared in embodiment 2 for the present invention；
Fig. 3 provides the electron microscope of the cobalt powder prepared in embodiment 3 for the present invention；
Fig. 4 provides the cobalt powder electron microscope prepared in contrast experiment for the present invention；
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of preparation method of spherical cobalt powder, specifically includes following steps：
Step 1, adds reactor to be reacted cobalt salt and ammonium bicarbonate solution cocurrent, controls course of reaction pH value so that half
System pH is adjusted to 7.0 ± 0.1 after hour；The cobalt salt be cobalt chloride, cobaltous sulfate, cobalt acetate in one kind, cobalt salt it is dense
It is 80-140g/l to spend, and flow is 1-2.5L/h；PH value is adjusted according to the flow of carbon ammonium；The concentration of carbon ammonium is 220g/l；
Step 2, keeps the pH value of step 1 constant, mixed solution is stirred, reacts and is precipitated；The temperature of reaction
It it is 40 DEG C, stir speed (S.S.) is 80-220r/min, the reaction time is 2h；
Step 3, the solution after being precipitated to step 2 carries out separation of solid and liquid and drying, obtains spherical cobaltous carbonate；
Step 4, the cobalt carbonate of step 3 is reduced in hydrogen atmosphere；
Reduction is carried out in push rod furnace, and the temperature of reduction is 280-430 DEG C, and the time of reduction is 3-8h, the flow of hydrogen
It is 400-1000L/h；
Step 5, the cobalt carbonate after step 4 is reduced carries out being cooled to 4-8h, that is, obtain spherical cobalt powder.
Compared compared with preparation method, the present invention mainly has following technical advantage：The cobalt powder of this technique productions is very thin
Primary particle reunite second particle, the size of these primary particles between 0.2-2 microns, averagely on 0.7 micron of left side
The right side, the size of second particle is between 3-6 microns, and AD and BET so use process, one than larger in hard alloy
Secondary particle can and carbide together ball milling and scatter, a size for cobalt granule of such practical function and tungsten carbide surface
Actually Nano grade, thus can and WC be sufficiently mixed, the efficiency and quality of mixing are improved, while increased hard alloy
Intensity.
Embodiment 1
By concentration for the cobalt chloride and concentration of 80g/l are the carbon ammonium hybrid reaction of 220g/l, the flow of wherein cobalt chloride is
2.5L/h, the flow that carbon ammonium is adjusted in course of reaction causes that the pH value of mixed solution after half an hour is 7.015, keeps pH value not
Become and continue to react, stirred at 40 DEG C, with the speed of 150r/min, precipitated after 2 hours of reaction, afterwards to the solution after precipitation
Separation of solid and liquid and drying are carried out, spherical cobaltous carbonate is obtained；Then cobalt carbonate is reduced in hydrogen atmosphere, the flow of hydrogen is
400L/h, the temperature of reduction is 350 DEG C, and the time of reduction is 4h, and the cobalt carbonate after reduction is cooled down into 4h afterwards, that is, obtain spherical
Cobalt powder.As shown in figure 1, the FSSS of cobalt powder is 1.28 μm, D50 is 5.56 μm.
Embodiment 2
By concentration for the cobalt chloride and concentration of 80g/l are the carbon ammonium hybrid reaction of 220g/l, the flow of wherein cobalt chloride is
2.5L/h, the flow that carbon ammonium is adjusted in course of reaction causes that the pH value of mixed solution after half an hour is 7.002, keeps pH value not
Become and continue to react, stirred at 40 DEG C, with the speed of 220r/min, precipitated after 2 hours of reaction, afterwards to the solution after precipitation
Separation of solid and liquid and drying are carried out, spherical cobaltous carbonate is obtained；Then cobalt carbonate is reduced in hydrogen atmosphere, the flow of hydrogen is
800L/h, the temperature of reduction is 350 DEG C, and the time of reduction is 3h, and the cobalt carbonate after reduction is cooled down into 6h afterwards, that is, obtain spherical
Cobalt powder.As shown in Fig. 2 the FSSS of cobalt powder is 0.96 μm, D50 is 4.811 μm.
Embodiment 3
By concentration for the cobalt chloride and concentration of 140g/l are the carbon ammonium hybrid reaction of 220g/l, the flow of wherein cobalt chloride is
1.42L/h, the flow that carbon ammonium is adjusted in course of reaction causes that the pH value of mixed solution after half an hour is 7.023, keeps pH value
It is constant to continue to react, stirred at 40 DEG C, with the speed of 80r/min, precipitated after 2 hours of reaction, afterwards to precipitation after it is molten
Liquid carries out separation of solid and liquid and drying, obtains spherical cobaltous carbonate；Then cobalt carbonate is reduced in hydrogen atmosphere, the flow of hydrogen is
1000L/h, the temperature of reduction is 350 DEG C, and the time of reduction is 8h, and the cobalt carbonate after reduction is cooled down into 3h afterwards, that is, obtain ball
Shape cobalt powder.As shown in figure 3, the FSSS of cobalt powder is 0.84 μm, D50 is 4.853 μm.
Contrast experiment：
By concentration for the cobalt chloride and concentration of 120g/l are the carbon ammonium hybrid reaction of 220g/l, the flow of wherein cobalt chloride is
2.5L/h, the flow of carbon ammonium is 4.6L/h, and pH value is 7.25, is stirred at 40 DEG C, with the speed of 220r/min, and reaction 2 is small
When after precipitate, separation of solid and liquid and drying are carried out to the solution after precipitation afterwards, obtain cobalt carbonate；Then by cobalt carbonate in hydrogen gas
Reduced in atmosphere, the flow of hydrogen is 1000L/h, and the temperature of reduction is 350, and the time of reduction is 8h, afterwards by the carbon after reduction
Sour cobalt row cools down 3h, that is, obtain cobalt powder.As shown in figure 4, gained cobalt powder dispersiveness and size distribution are poor, hardly balling-up.
The above, only presently preferred embodiments of the present invention is not intended to limit the scope of the present invention.
Claims (10)
1. a kind of preparation method of spherical cobalt powder, it is characterised in that specifically implement according to following steps：
Step 1, adds reactor to be reacted cobalt salt and ammonium bicarbonate solution cocurrent, controls course of reaction pH value so that half an hour
System pH is adjusted to 7.0 ± 0.1 afterwards；
Step 2, continues cocurrent and adds cobalt salt and ammonium bicarbonate solution, keeps the pH value of step 1 constant, continues to react and precipitates；
Step 3, the solution after being precipitated to step 2 carries out separation of solid and liquid and drying, obtains spherical cobaltous carbonate；
Step 4, the cobalt carbonate of step 3 is reduced in hydrogen atmosphere；
Step 5, the cobalt carbonate after step 4 is reduced is cooled down, that is, obtain spherical cobalt powder.
2. a kind of preparation method of spherical cobalt powder according to claim 1, it is characterised in that the cobalt salt in the step 1
It is the one kind in cobalt chloride, cobaltous sulfate, cobalt acetate.
3. a kind of preparation method of spherical cobalt powder according to claim 2, it is characterised in that cobalt salt in the step 1
Concentration is 80-140g/l, and flow is 1-2.5L/h.
4. a kind of preparation method of spherical cobalt powder according to claim 3, it is characterised in that the pH value in the step 1
Flow according to carbon ammonium is adjusted.
5. a kind of preparation method of spherical cobalt powder according to claim 4, it is characterised in that carbon ammonium in the step 1
Concentration is 220g/l.
6. the preparation method of a kind of spherical cobalt powder according to claim 5, it is characterised in that reacted in the step 2
Temperature is 40 DEG C, and the time of reaction is 1-5h.
7. a kind of preparation method of spherical cobalt powder according to claim 6, it is characterised in that the stirring in the step 2
Speed is 80-220r/min.
8. a kind of preparation method of spherical cobalt powder according to claim 7, it is characterised in that the reduction in the step 4
Carried out in push rod furnace, the temperature of reduction is 280-430 DEG C, the time of reduction is 3-8h.
9. a kind of preparation method of spherical cobalt powder according to claim 8, it is characterised in that hydrogen in the step 4
Flow is 400-1000L/h.
10. the preparation method of a kind of spherical cobalt powder according to claim 9, it is characterised in that cooled down in the step 5
Time is 4-8h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107649689A (en) * | 2017-11-07 | 2018-02-02 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of super-fine cobalt powder |
| CN114074187A (en) * | 2020-08-21 | 2022-02-22 | 荆门市格林美新材料有限公司 | Preparation method of large FSSS and large-particle-size spherical cobalt powder |
| CN114230456A (en) * | 2021-12-24 | 2022-03-25 | 马鞍山昂扬新材料科技有限公司 | Synthesis process of cobalt acetate |
| CN114535590A (en) * | 2022-01-24 | 2022-05-27 | 安徽寒锐新材料有限公司 | Method for preparing cobalt powder from cobalt carbonate |
| CN114905048A (en) * | 2022-06-02 | 2022-08-16 | 兰州理工大学 | Preparation method of nano cobalt powder for additive manufacturing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102910686A (en) * | 2011-08-04 | 2013-02-06 | 深圳市格林美高新技术股份有限公司 | Cobalt carbonate preparation method and superfine cobalt powder preparation method |
| CN104722766A (en) * | 2013-12-18 | 2015-06-24 | 深圳市格林美高新技术股份有限公司 | High-density cobalt powder and synthetic method thereof |
| CN105800699A (en) * | 2016-04-20 | 2016-07-27 | 湖南海纳新材料有限公司 | Method for preparing high-sphericity-degree and large-particle cobaltosic oxide |
| CN105935779A (en) * | 2016-06-22 | 2016-09-14 | 荆门市格林美新材料有限公司 | Cobalt powder preparing method |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102910686A (en) * | 2011-08-04 | 2013-02-06 | 深圳市格林美高新技术股份有限公司 | Cobalt carbonate preparation method and superfine cobalt powder preparation method |
| CN104722766A (en) * | 2013-12-18 | 2015-06-24 | 深圳市格林美高新技术股份有限公司 | High-density cobalt powder and synthetic method thereof |
| CN105800699A (en) * | 2016-04-20 | 2016-07-27 | 湖南海纳新材料有限公司 | Method for preparing high-sphericity-degree and large-particle cobaltosic oxide |
| CN105935779A (en) * | 2016-06-22 | 2016-09-14 | 荆门市格林美新材料有限公司 | Cobalt powder preparing method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107649689A (en) * | 2017-11-07 | 2018-02-02 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of super-fine cobalt powder |
| CN114074187A (en) * | 2020-08-21 | 2022-02-22 | 荆门市格林美新材料有限公司 | Preparation method of large FSSS and large-particle-size spherical cobalt powder |
| CN114230456A (en) * | 2021-12-24 | 2022-03-25 | 马鞍山昂扬新材料科技有限公司 | Synthesis process of cobalt acetate |
| CN114535590A (en) * | 2022-01-24 | 2022-05-27 | 安徽寒锐新材料有限公司 | Method for preparing cobalt powder from cobalt carbonate |
| CN114905048A (en) * | 2022-06-02 | 2022-08-16 | 兰州理工大学 | Preparation method of nano cobalt powder for additive manufacturing |
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