CN112355317A - Preparation method of superfine spherical cobalt powder - Google Patents
Preparation method of superfine spherical cobalt powder Download PDFInfo
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- CN112355317A CN112355317A CN202011127817.7A CN202011127817A CN112355317A CN 112355317 A CN112355317 A CN 112355317A CN 202011127817 A CN202011127817 A CN 202011127817A CN 112355317 A CN112355317 A CN 112355317A
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000011261 inert gas Substances 0.000 claims abstract description 32
- 238000001354 calcination Methods 0.000 claims abstract description 27
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 claims abstract description 19
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 18
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 18
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 18
- ZJRWDIJRKKXMNW-UHFFFAOYSA-N carbonic acid;cobalt Chemical compound [Co].OC(O)=O ZJRWDIJRKKXMNW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 16
- 239000010941 cobalt Substances 0.000 claims abstract description 16
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims abstract description 15
- 230000001681 protective effect Effects 0.000 claims abstract description 15
- 229910021446 cobalt carbonate Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 13
- 239000002244 precipitate Substances 0.000 claims abstract description 12
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 10
- 150000001868 cobalt Chemical class 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000012266 salt solution Substances 0.000 claims abstract description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000012716 precipitator Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 54
- 238000006722 reduction reaction Methods 0.000 claims description 31
- 229910052757 nitrogen Inorganic materials 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 238000010902 jet-milling Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 11
- 239000000843 powder Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000000956 alloy Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000002243 precursor Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 description 1
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000009692 water atomization Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
Abstract
The invention relates to the technical field of cobalt-based powder material preparation, in particular to a preparation method of superfine spherical cobalt powder. The method comprises the following steps: (1) reacting a cobalt salt solution with an ammonium bicarbonate or sodium carbonate precipitator under a heating condition to obtain a cobalt carbonate precipitate; (2) filtering, washing with pure water and drying the cobalt carbonate precipitate to obtain cobalt carbonate powder; (3) placing the cobalt carbonate powder into a calcining furnace, and heating and decomposing the cobalt carbonate powder in an anaerobic state to obtain cobaltous oxide; (4) placing cobaltous oxide powder obtained by calcination and decomposition into a reduction furnace, and introducing hydrogen to reduce to obtain loose sponge cobalt blocks; (5) and (3) carrying out airflow crushing on the spongy cobalt block under the protective atmosphere of closed-loop circulating inert gas to obtain the superfine spherical cobalt powder with the Fisher particle size of 0.4-0.8 mu m. The prepared cobalt powder has the advantages of superfine granularity, spherical shape, uniform and controllable particle size, uniform particle size distribution, good flow property and the like.
Description
Technical Field
The invention relates to the technical field of cobalt-based powder material preparation, in particular to a preparation method of superfine spherical cobalt powder.
Background
Cobalt powder is widely used in high temperature alloy, hard alloy, diamond tool, battery industry and magnetic material industry. In recent years, with the rapid development of process technology in the downstream alloy industry, the demand for cobalt powder is increasing, and the quality requirement is becoming strict. At present, a plurality of methods for preparing cobalt powder at home and abroad mainly comprise a hydrogen reduction method, an oxalate thermal decomposition method, a water atomization method, an electrolysis method, a polyol liquid phase reduction method and the like. The hydrogen reduction method is relatively suitable for industrial mass production due to the relatively simple process flow, and is the mainstream method for producing the cobalt powder for the alloy tool at home and abroad in a large scale at present.
For a long time, the hydrogen reduction method is mainly used for preparing the superfine cobalt powder by synchronously decomposing and reducing cobalt salts such as precursor cobalt carbonate or cobalt oxalate and the like, the preparation method has the advantage of short preparation process, but the particle size of cobalt powder particles is larger due to the synchronous crystal nucleation and growth of the cobalt powder when the cobalt salts are synchronously decomposed and reduced, the method is suitable for producing the cobalt powder with the Fisher particle size of more than 1.0 mu m, and the superfine cobalt powder with the Fisher particle size range of 0.4-0.8 mu m is basically difficult to produce.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of superfine spherical cobalt powder with a Fisher size range of 0.4-0.8 mu m.
In order to achieve the above object, the preparation method of ultrafine spherical cobalt powder of the present invention comprises the following steps:
(1) reacting a cobalt salt solution with an ammonium bicarbonate or sodium carbonate precipitator under a heating condition to obtain a cobalt carbonate precipitate;
(2) filtering, washing with pure water and drying the cobalt carbonate precipitate to obtain cobalt carbonate powder;
(3) placing the cobalt carbonate powder into a calcining furnace, heating and decomposing the cobalt carbonate powder in an oxygen-free state to obtain cobaltous oxide, introducing protective inert gas with the micro-positive pressure of 10-25 Pa into the calcining furnace, wherein the thermal decomposition temperature is 200-350 ℃, and the calcining time is 1-2 hours;
(4) heating the reduction furnace to 350-480 ℃, wherein the inlet flow rate is 2.8-4.0m3And h, hydrogen gas, putting cobaltous oxide into a reduction furnace for reaction for 2.5-4.5 h, and cooling the reduction product for 2.5-3.0 h to normal temperature through a cooling circulation water jacket filled with inert gas for protection after the reduction reaction is finished to obtain loose spongy cobalt blocks.
(5) And (3) carrying out airflow crushing on the spongy cobalt block under the protective atmosphere of closed-loop circulating inert gas to obtain the superfine spherical cobalt powder with the Fisher particle size of 0.4-0.8 mu m.
Preferably, the cobalt salt solution in the step (1) is a cobalt chloride solution, the concentration of the cobalt chloride solution is 90-140 g/L, the concentration of ammonium bicarbonate or sodium carbonate is 180-220 g/L, the heating temperature is 40-50 ℃, and the pH value of the reaction end point is 6.8-7.3.
Preferably, ammonium bicarbonate is selected as the precipitating agent in step (1).
The drying mode in the step (2) is one of drying in a box furnace, flash drying and the like;
preferably, the drying manner selected in step (2) is flash drying.
The calcination decomposition in the step (3) can be realized by heating equipment such as a rotary kiln, a plate furnace and the like;
preferably, the calcining equipment selected in step (3) is a rotary kiln.
The protective inert gas in the calcining decomposition process in the step (3) is nitrogen or argon;
preferably, the protective inert gas selected in step (3) is nitrogen.
The reduction furnace in the step (4) is one of a steel belt type reduction furnace, a tubular furnace, a push boat furnace and the like;
preferably, the reduction furnace selected in step (4) is a steel strip type reduction furnace.
The protective inert gas in the cooling process in the step (4) is carbon dioxide, nitrogen, argon or mixed inert gas;
preferably, the protective inert gas selected in step (4) is a mixed gas of carbon dioxide and nitrogen, wherein the volume ratio of the nitrogen is 70-80%.
The inert gas selected in the step (5) is one of nitrogen, argon and the like, the dew point of the inert gas is less than minus 25 ℃, and the jet milling grinding pressure is 0.60-0.85 MPa;
preferably, the inert gas selected in step (5) is nitrogen.
The invention has the following beneficial effects:
the method adopts low-temperature pre-calcination decomposition to prepare cobaltous oxide as a precursor of cobalt powder, and then performs hydrogen reduction to prepare cobalt powder, is a preparation method which is different from the method of directly putting cobalt carbonate into a reduction furnace and introducing hydrogen to perform decomposition and reduction simultaneously, and the prepared cobalt powder has the advantages of superfine granularity, spherical shape, uniform and controllable particle size distribution, good fluidity and the like.
Experiments prove that the cobaltous carbonate can be subjected to decomposition reaction at a lower calcining temperature to obtain cobaltous oxide (+ 2-valent cobalt), the cobaltous oxide obtained by decomposition is easy to be subjected to oxidation reaction with oxygen in the air to generate cobaltous oxide (+ 3-valent cobalt), the reaction speed is in positive correlation with the calcining temperature, and the higher the degree of cobaltous oxide oxidized into cobaltous oxide is along with the increase of the calcining temperature, the particle size can be increased, so that the cobalt powder prepared by hydrogen reduction at the rear end has larger particle size, and in addition, the cobalt oxide with the valence of +3 needs longer reduction time and larger hydrogen consumption when reduced, so that the higher calcining temperature is not favorable for preparing cobalt powder precursor cobaltous oxide with the requirement of superfine particle size.
Drawings
FIG. 1 is a schematic view of the process flow of the preparation method of ultrafine spherical cobalt powder of the present invention.
FIG. 2 is an SEM photograph (magnification of 5000) of a product obtained in example 1 of the present invention.
FIG. 3 is an SEM photograph (magnification of 5000) of a product obtained in example 2 of the present invention.
FIG. 4 is an SEM photograph (magnification of 5000) of a product obtained in example 3 of the present invention.
Detailed Description
Example 1
Step 1: respectively preparing an ammonium bicarbonate solution and a cobalt chloride solution by using pure water, wherein the concentration of the ammonium bicarbonate solution is 180g/L, the concentration of the cobalt chloride solution is 90g/L, putting the ammonium bicarbonate solution into a reaction kettle, heating to 44 ℃, then dropwise adding the cobalt chloride solution into the reaction kettle under the conditions of stirring and heat preservation to react with the ammonium bicarbonate to synthesize a cobalt carbonate precipitate, and the pH value at the end of the reaction is 6.8.
Step 2: washing and slurrying the cobalt carbonate precipitate by using pure water at 70 ℃, and drying by using a flash evaporation drying furnace to obtain cobalt carbonate powder, wherein the drying temperature is 120 ℃.
And step 3: putting the cobalt carbonate powder into a rotary kiln, heating and decomposing the cobalt carbonate powder in an oxygen-free state to obtain cobaltous oxide, introducing protective inert gas nitrogen with the micro-positive pressure of 10Pa into the calcining furnace, wherein the calcining decomposition temperature is 200 ℃, and the calcining time is 1.6 h.
And 4, step 4: putting cobaltous oxide into a steel belt type reduction furnace, heating the reduction furnace to 360 ℃, and introducing hydrogen with the flow rate of 3.8m3The reaction time is 4.0 h; and after the reduction reaction is finished, cooling the reduction product for 2.5 hours to normal temperature through a cooling circulation water jacket filled with inert gas for protection to obtain loose spongy cobalt blocks, wherein the inert gas is a mixed gas of carbon dioxide and nitrogen, and the volume ratio of the nitrogen is 80%.
And 5: crushing the spongy cobalt block by using a closed-loop circulating inert gas nitrogen protection jet mill to obtain cobalt powder, wherein the crushing and grinding pressure is 0.70MPa, and the dew point of compressed nitrogen is lower than minus 25 ℃. The Fisher size of the cobalt powder obtained by jet milling is 0.53 mu m, and the microscopic morphology of the cobalt powder is spherical as can be seen from a Scanning Electron Microscope (SEM) figure 2.
Example 2
Step 1: respectively preparing an ammonium bicarbonate solution and a cobalt chloride solution by using pure water, wherein the concentration of the ammonium bicarbonate solution is 190g/L, the concentration of the cobalt chloride solution is 95g/L, putting the ammonium bicarbonate solution into a reaction kettle, heating to 44 ℃, then dropwise adding the cobalt chloride solution into the reaction kettle under the conditions of stirring and heat preservation to react with the ammonium bicarbonate to synthesize a cobalt carbonate precipitate, and the pH value at the end of the reaction is 6.9.
Step 2: washing and slurrying the cobalt carbonate precipitate by using pure water at 75 ℃, and drying by using a flash evaporation drying furnace to obtain cobalt carbonate powder, wherein the drying temperature is 120 ℃.
And step 3: putting the cobalt carbonate powder into a rotary kiln, heating and decomposing the cobalt carbonate powder in an oxygen-free state to obtain cobaltous oxide, introducing protective inert gas nitrogen with the micro-positive pressure of 14Pa into the calcining furnace, wherein the calcining decomposition temperature is 240 ℃, and the calcining time is 1.5 h.
And 4, step 4: putting cobaltous oxide into a steel belt type reducing furnace, heating the reducing furnace to 400 ℃, and introducing hydrogen with the flow rate of 3.4m3H, the reaction time is 3.5 h; and after the reduction reaction is finished, cooling the reduction product for 2.7 hours to normal temperature through a cooling circulation water jacket filled with inert gas for protection to obtain loose spongy cobalt blocks, wherein the inert gas is a mixed gas of carbon dioxide and nitrogen, and the volume ratio of the nitrogen is 75%.
And 5: crushing the spongy cobalt block by using a closed-loop circulating inert gas nitrogen protection jet mill to obtain cobalt powder, wherein the crushing and grinding pressure is 0.75MPa, and the dew point of compressed nitrogen is lower than minus 25 ℃. The Fisher size of the cobalt powder obtained by jet milling is 0.55 mu m, and the microscopic morphology of the cobalt powder is spherical as can be seen from a Scanning Electron Microscope (SEM) figure 3.
Example 3
Step 1: respectively preparing an ammonium bicarbonate solution and a cobalt chloride solution by using pure water, wherein the concentration of the ammonium bicarbonate solution is 200g/L, the concentration of the cobalt chloride solution is 120g/L, putting the ammonium bicarbonate solution into a reaction kettle, heating to 46 ℃, then dropwise adding the cobalt chloride solution into the reaction kettle under the conditions of stirring and heat preservation to react with the ammonium bicarbonate to synthesize a cobalt carbonate precipitate, and the pH value at the end of the reaction is 7.0.
Step 2: washing and slurrying the cobalt carbonate precipitate by using pure water at the temperature of 80 ℃, and drying by using a flash evaporation drying furnace to obtain cobalt carbonate powder, wherein the drying temperature is 120 ℃.
And step 3: putting the cobalt carbonate powder into a rotary kiln, heating and decomposing the cobalt carbonate powder in an oxygen-free state to obtain cobaltous oxide, introducing protective inert gas nitrogen with the micro-positive pressure of 18Pa into the calcining furnace, wherein the calcining decomposition temperature is 300 ℃, and the calcining time is 1.2 h.
And 4, step 4: putting cobaltous oxide into a steel belt type reducing furnace, heating the reducing furnace to 450 ℃, and introducing hydrogen with the flow rate of 3.0m3H, the reaction time is 3.2 h; and after the reduction reaction is finished, cooling the reduction product for 3.0h to normal temperature through a cooling circulation water jacket filled with inert gas for protection to obtain loose spongy cobalt blocks, wherein the inert gas is a mixed gas of carbon dioxide and nitrogen, and the volume ratio of the nitrogen is 70%.
And 5: crushing the spongy cobalt block by using a closed-loop circulating inert gas nitrogen protection jet mill to obtain cobalt powder, wherein the crushing and grinding pressure is 0.80MPa, and the dew point of compressed nitrogen is lower than minus 25 ℃. The Fisher size of the cobalt powder obtained by jet milling is 0.61 μm, and the microscopic morphology of the cobalt powder is spherical as can be seen from a Scanning Electron Microscope (SEM) image 4.
Claims (9)
1. A preparation method of superfine spherical cobalt powder is characterized by comprising the following steps: the method comprises the following steps:
(1) reacting a cobalt salt solution with an ammonium bicarbonate or sodium carbonate precipitator under a heating condition to obtain a cobalt carbonate precipitate;
(2) filtering, washing with pure water and drying the cobalt carbonate precipitate to obtain cobalt carbonate powder;
(3) placing the cobalt carbonate powder into a calcining furnace, heating and decomposing the cobalt carbonate powder in an oxygen-free state to obtain cobaltous oxide, introducing protective inert gas with the micro-positive pressure of 10-25 Pa into the calcining furnace, wherein the thermal decomposition temperature is 200-350 ℃, and the calcining time is 1-2 hours;
(4) heating the reduction furnace to 350-480 ℃, and introducing the gas with the flow of 2.8-4.0 m3And h, hydrogen gas, putting cobaltous oxide into a reduction furnace for reaction for 2.5-4.5 h, and cooling the reduction product for 2.5-3.0 h to normal temperature through a cooling circulation water jacket filled with inert gas for protection after the reduction reaction is finished to obtain loose spongy cobalt blocks.
(5) And (3) carrying out airflow crushing on the spongy cobalt block under the protective atmosphere of closed-loop circulating inert gas to obtain the superfine spherical cobalt powder with the Fisher particle size of 0.4-0.8 mu m.
2. The method for preparing ultrafine spherical cobalt powder according to claim 1, wherein the method comprises the following steps: the cobalt salt solution in the step (1) is a cobalt chloride solution, the concentration of the cobalt chloride solution is 90-140 g/L, the concentration of ammonium bicarbonate or sodium carbonate is 180-220 g/L, the heating temperature is 40-50 ℃, and the pH value of the reaction end point is 6.8-7.3.
3. The method for preparing ultrafine spherical cobalt powder according to claim 1, wherein the method comprises the following steps: and (3) drying in the step (2) by a box furnace or flash evaporation.
4. The method for preparing ultrafine spherical cobalt powder according to claim 1, wherein the method comprises the following steps: the calcining furnace in the step (3) is a rotary kiln or a plate furnace.
5. The method for preparing ultrafine spherical cobalt powder according to claim 1 or 2, characterized in that: and (3) the protective inert gas in the calcining decomposition process is nitrogen or argon.
6. The method for preparing ultrafine spherical cobalt powder according to claim 1, wherein the method comprises the following steps: and (4) the reduction furnace is a steel belt type reduction furnace, a tubular furnace or a push boat furnace.
7. The method for preparing ultrafine spherical cobalt powder according to claim 1 or 6, wherein: and (4) the protective inert gas in the cooling process in the step (4) is one or more of carbon dioxide, nitrogen and argon.
8. The method for preparing ultrafine spherical cobalt powder according to claim 7, wherein the method comprises the following steps: the protective inert gas in the cooling process selected in the step (4) is a mixed gas of carbon dioxide and nitrogen, wherein the volume ratio of the nitrogen is 70-80%.
9. The method for preparing ultrafine spherical cobalt powder according to claim 1, wherein the method comprises the following steps: and (3) selecting the inert gas in the step (5) as nitrogen or argon, wherein the dew point of the inert gas is less than minus 25 ℃, and the jet milling grinding pressure is 0.60-0.85 MPa.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113664216A (en) * | 2021-08-13 | 2021-11-19 | 衢州华友钴新材料有限公司 | Preparation method of large-particle-size spherical cobalt powder |
| CN113909485A (en) * | 2021-10-11 | 2022-01-11 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
| CN114406277A (en) * | 2021-12-22 | 2022-04-29 | 荆门市格林美新材料有限公司 | Preparation method of small-Fisher-size cobalt powder |
| 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 |
| CN114804221A (en) * | 2022-04-28 | 2022-07-29 | 荆门市格林美新材料有限公司 | Cobaltous oxide and preparation method and application thereof |
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| 曲选辉: "《粉末冶金原理与工艺》", 31 May 2013, 冶金工业出版社 * |
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| CN113909485B (en) * | 2021-10-11 | 2023-11-17 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
| CN114406277A (en) * | 2021-12-22 | 2022-04-29 | 荆门市格林美新材料有限公司 | Preparation method of small-Fisher-size cobalt powder |
| 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 |
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