CN100374231C - Preparation method of nano-cobalt powder - Google Patents
Preparation method of nano-cobalt powder Download PDFInfo
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- CN100374231C CN100374231C CNB2006100671641A CN200610067164A CN100374231C CN 100374231 C CN100374231 C CN 100374231C CN B2006100671641 A CNB2006100671641 A CN B2006100671641A CN 200610067164 A CN200610067164 A CN 200610067164A CN 100374231 C CN100374231 C CN 100374231C
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000007921 spray Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 claims abstract description 7
- WRWZNPYXEXPBAY-UHFFFAOYSA-N azane cobalt Chemical compound N.[Co] WRWZNPYXEXPBAY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 208000032544 Cicatrix Diseases 0.000 claims description 6
- 231100000241 scar Toxicity 0.000 claims description 6
- 230000037387 scars Effects 0.000 claims description 6
- 238000005352 clarification Methods 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 14
- 238000004108 freeze drying Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000004663 powder metallurgy Methods 0.000 abstract 1
- 229910017052 cobalt Inorganic materials 0.000 description 8
- 239000010941 cobalt Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 239000000956 alloy Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000007670 refining Methods 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 battery Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910000498 pewter Inorganic materials 0.000 description 1
- 239000010957 pewter Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention belongs to the field of powder metallurgy. No relevant report on the research of nanometer cobalt powder preparation by the freeze drying technology exists home and abroad up to now. The present invention comprises: cobalt oxalate CoC2O4.2H2O crystal powder is dissolved in ammonia water to obtain a clear cobalt-ammonia complex compound solution; a universal nitrogen spray gun is used for dispersing the clear solution in liquid nitrogen to be prefreezed; the congelation prefreezed in the liquidnitrogen nitrogen is put in a freezedryer for vacuum drying to obtain precursors; the dried precursors are treated by hydrogen reduction, the hydrogen flow rate is 0.1 to 0.3 m3 / hr, the reduction is carried out at the temperature of 200 DEG C to 400 DEG C, and the temperature is preserved for 2 to 8 hours to obtain nanometer cobalt powder. The present invention has the advantages of simple technology, low equipment requirement, cheap and easy obtained raw material and greatly reduced energy consumption due to the reduction temperature of about 300 DEG C lower than that of the ordinary industrial method. The prepared cobalt powder has the advantages of good dispersancy, narrow particle size distribution, no need of surface active agent and avoidance of the introduction of impurity elements.
Description
Technical field
A kind of preparation method of nano-cobalt powder belongs to powder metallurgical technology.
Background technology
Cobalt, hard, malleable pewter metal is rich in gloss.Abundance is 0.0025% in the earth's crust.China is world's second largest cobalt producing country, it also is the second largest country of consumption of refining cobalt, 1998 to 2004 according to statistics, the annual average rate of increase of China's refining cobalt consumption figure is 20.7%, refining cobalt consumption figure reached 9500 tons in 2004, and wherein battery industry is first consumer field, accounts for 57%, the colour glaze industry accounts for 14%, and magnetic material accounts for 8%.Japan is the big cobalt of the first in the world country of consumption, and 60% is used in field of batteries, the third-largest cobalt country of consumption U.S., and 55% is used to make super carbide alloy.
Super-fine cobalt powder shows the performance of many excellences owing to its special physics, chemical property in the application in fields such as carbide alloy, battery, catalyst, magnetic material, absorbing material, pottery.For example, make the permanent magnetism recording materials, can make the packing density of tape and soft or hard dish improve tens of times, and can improve their fidelity performance significantly with super-fine cobalt powder.Simultaneously because super-fine cobalt powder to electromagnetic special absorption, can be used as military high-performance millimeter wave stealth material, visible light, infrared ray stealth material and structural formula stealth material, mobile phone radiation shielding material.The super-fine cobalt powder that uses aspect carbide alloy makes it have higher wearability and crack resistance because cross-breaking strength, hardness and the density of alloy all are improved.If can be at cobalt powder particularly in the preparation of super-fine cobalt powder with use and get along with, to making full use of resource, increasing economic efficiency, shorten and developed country between gap all significant.
The result of literature survey shows that Freeze Drying Technique prepares the research of nano-cobalt powder, does not also have relevant report so far both at home and abroad.
Summary of the invention
Adopt the present invention to prepare nano-cobalt powder, its technology is very simple, and is low for equipment requirements, and raw material cheaply is easy to get.Reduction temperature of the present invention hangs down about 300 ℃ than the reduction temperature of common industry law, greatly reduces energy consumption.Cobalt powder good dispersion, narrow particle size distribution, the pattern prepared are even, and do not need to add surfactant, have avoided the introducing of impurity element.
The preparation method of a kind of nano-cobalt powder provided by the present invention is characterized in that: it may further comprise the steps:
1) with cobalt oxalate [CoC
2O42H
2O] crystal powder is dissolved in the ammoniacal liquor cobalt ammonia complex solution that must clarify;
2) use general nitrogen spray gun, above-mentioned settled solution is dispersed in pre-freeze in the liquid nitrogen;
3) scars after the pre-freeze in the above-mentioned liquid nitrogen are placed freeze dryer carry out vacuum drying and obtain presoma;
4) above-mentioned dried presoma is carried out hydrogen reducing, hydrogen flowing quantity is 0.1 cubic metre/hour～0.3 cubic metre/hour, and 200 ℃～400 ℃ reduction are incubated 2 hours～8 hours and obtain nano-cobalt powder.
Step 2) described nitrogen spray gun, its pressure is 1.5 atmospheric pressure～3.5 atmospheric pressure.
The described vacuum drying of step 3), wherein the performing a programme of freeze dryer is: the operating pressure in 0 minute～2000 minutes is that 450 millitorrs, temperature are-20 ℃; Operating pressure in 2000 minutes～3700 minutes is that 300 millitorrs, temperature are-11 ℃; Operating pressure in 3700 minutes～5000 minutes is that 150 millitorrs, temperature are-6 ℃; Operating pressure in 5000 minutes～5800 minutes is that 80 millitorrs, temperature are 0 ℃; Operating pressure in 5800 minutes～6000 minutes is that 5 millitorrs, temperature are 15 ℃.
The present invention adopts liquid nitrogen pre-freeze-freeze-drying, can prevent the poly-partially and crystallization of solution component, obtains amorphous powder simultaneously.By the low temperature hydrogen reduction, obtain the cobalt powder of nano level crystallite dimension again.
Can know that from the X diffracting spectrum of Fig. 1 the thing phase composition of final products only has cobalt.
From the image of the field emission scanning electron microscope of Fig. 2 as can be seen, the powder size distribution that adopts the method for liquid nitrogen pre-freeze-freeze drying-hydrogen reducing to obtain is even, and particle is about the powder of 40-50nm.
Hence one can see that, and with the obvious refinement of powder crystal grain of desivac preparation, size reaches nanoscale, thereby can improve surface-active, surperficial purity, specific area, has great skin effect and bulk effect.
Description of drawings
Fig. 1: the nano-powder X diffracting spectrum of preparation method's example 1 of the present invention;
Fig. 2: the nano-powder FESEM picture of preparation method's example 1 of the present invention;
The specific embodiment
Example 1: get cobalt oxalate [CoC
2O42H
2O] pink crystal powder 50 grams are dissolved in 250 milliliters of ammoniacal liquor and get the brown settled solution.Use the nitrogen spray gun, spray gun pressure is 3.5 atmospheric pressure, and the mixed solution of clarifying is dispersed in the liquid nitrogen.Scars with liquid nitrogen frozen place the FTD Dura-stop MP of FTS company type freeze dryer to carry out vacuum drying again, and the performing a programme of freeze dryer is: the operating pressure in 0 minute～2000 minutes is that 450 millitorrs, temperature are-20 ℃; Operating pressure in 2000 minutes～3700 minutes is that 300 millitorrs, temperature are-11 ℃; Operating pressure in 3700 minutes～5000 minutes is that 150 millitorrs, temperature are-6 ℃; Operating pressure in 5000 minutes～5800 minutes is that 80 millitorrs, temperature are 0 ℃; Operating pressure in 5800 minutes～6000 minutes is that 5 millitorrs, temperature are 15 ℃.Adopt the presoma of hydrogen reducing freeze-drying, hydrogen flowing quantity is 0.3 cubic metre/hour, and 200 ℃ of reduction temperatures are incubated 7 hours, obtain the nano-cobalt powder that crystallite dimension is 45.5nm.
Example 2: get cobalt oxalate [CoC
2O
42H
2O] pink crystal powder 50 grams are dissolved in 250 milliliters of ammoniacal liquor and get the brown settled solution.Use the nitrogen spray gun, spray gun pressure is 1.5 atmospheric pressure, and the mixed solution of clarifying is dispersed in the liquid nitrogen.Scars with liquid nitrogen frozen place the FTD Dura-stop MP of FTS company type freeze dryer to carry out vacuum drying again, and the performing a programme of freeze dryer is: the operating pressure in 0 minute～2000 minutes is that 450 millitorrs, temperature are-20 ℃; Operating pressure in 2000 minutes～3700 minutes is that 300 millitorrs, temperature are-11 ℃; Operating pressure in 3700 minutes～5000 minutes is that 150 millitorrs, temperature are-6 ℃; Operating pressure in 5000 minutes～5800 minutes is that 80 millitorrs, temperature are 0 ℃; Operating pressure in 5800 minutes～6000 minutes is that 5 millitorrs, temperature are 15 ℃.Adopt the presoma of hydrogen reducing freeze-drying, hydrogen flowing quantity is 0.1 cubic metre/hour, and 400 ℃ of reduction temperatures are incubated 2 hours, obtain the nano-cobalt powder that crystallite dimension is 57.3nm.
Example 3: get cobalt oxalate [CoC
2O
42H
2O] pink crystal powder 50 grams are dissolved in 250 milliliters of ammoniacal liquor and get the brown settled solution.Use the nitrogen spray gun, spray gun pressure is 2.5 atmospheric pressure, and the mixed solution of clarifying is dispersed in the liquid nitrogen.Scars with liquid nitrogen frozen place the FTD Dura-stop MP of FTS company type freeze dryer to carry out vacuum drying again, and the performing a programme of freeze dryer is: the operating pressure in 0 minute～2000 minutes is that 450 millitorrs, temperature are-20 ℃; Operating pressure in 2000 minutes～3700 minutes is that 300 millitorrs, temperature are-11 ℃; Operating pressure in 3700 minutes～5000 minutes is that 150 millitorrs, temperature are-6 ℃; Operating pressure in 5000 minutes～5800 minutes is that 80 millitorrs, temperature are 0 ℃; Operating pressure in 5800 minutes～6000 minutes is that 5 millitorrs, temperature are 15 ℃.Adopt the presoma of hydrogen reducing freeze-drying, hydrogen flowing quantity is 0.2 cubic metre/hour, and 300 ℃ of reduction temperatures are incubated 2 hours, obtain the nano-cobalt powder that crystallite dimension is 40.7nm.
Example 4: get cobalt oxalate [CoC
2O
42H
2O] pink crystal powder 50 grams are dissolved in 250 milliliters of ammoniacal liquor and get the brown settled solution.Use the nitrogen spray gun, spray gun pressure is 2.0 atmospheric pressure, and the mixed solution of clarifying is dispersed in the liquid nitrogen.Scars with liquid nitrogen frozen place the FTD Dura-stop MP of FTS company type freeze dryer to carry out vacuum drying again, and the performing a programme of freeze dryer is: the operating pressure in 0 minute～2000 minutes is that 450 millitorrs, temperature are-20 ℃; Operating pressure in 2000 minutes～3700 minutes is that 300 millitorrs, temperature are-11 ℃; Operating pressure in 3700 minutes～5000 minutes is that 150 millitorrs, temperature are-6 ℃; Operating pressure in 5000 minutes～5800 minutes is that 80 millitorrs, temperature are 0 ℃; Operating pressure in 5800 minutes～6000 minutes is that 5 millitorrs, temperature are 15 ℃.Adopt the presoma of hydrogen reducing freeze-drying, hydrogen flowing quantity is 0.3 cubic metre/hour, and 250 ℃ of reduction temperatures are incubated 5 hours, obtain the nano-cobalt powder that crystallite dimension is 52.7nm.
Claims (3)
1. the preparation method of a nano-cobalt powder is characterized in that, it may further comprise the steps:
1) with cobalt oxalate CoC
2O
42H
2The O crystal powder is dissolved in the ammoniacal liquor, the cobalt ammonia complex solution that must clarify;
2) use general nitrogen spray gun, the cobalt ammonia complex solution of above-mentioned clarification is dispersed in pre-freeze in the liquid nitrogen;
3) scars after the pre-freeze in the above-mentioned liquid nitrogen are placed freeze dryer carry out vacuum drying and obtain presoma;
4) above-mentioned dried presoma is carried out hydrogen reducing, hydrogen flowing quantity is 0.1 cubic metre/hour～0.3 cubic metre/hour, and 200 ℃～400 ℃ reduction are incubated 2 hours～8 hours and obtain nano-cobalt powder.
2. nano-cobalt powder preparation method according to claim 1 is characterized in that: step 2) described pre-freeze, nitrogen spray gun wherein, its pressure is 1.5 atmospheric pressure～3.5 atmospheric pressure.
3. nano-cobalt powder preparation method according to claim 1 is characterized in that: the described vacuum drying of step 3), and wherein the performing a programme of freeze dryer is: the operating pressure in 0 minute～2000 minutes is that 450 millitorrs, temperature are-20 ℃; Operating pressure in 2000 minutes～3700 minutes is that 300 millitorrs, temperature are-11 ℃; Operating pressure in 3700 minutes～5000 minutes is that 150 millitorrs, temperature are-6 ℃; Operating pressure in 5000 minutes～5800 minutes is that 80 millitorrs, temperature are 0 ℃; Operating pressure in 5800 minutes～6000 minutes is that 5 millitorrs, temperature are 15 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102049525B (en) * | 2009-10-29 | 2012-08-29 | 北京有色金属研究总院 | Preparation method of spherical nanometer cobalt alloy powder containing transition metal elements |
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| CN101780545B (en) * | 2010-01-18 | 2013-03-27 | 深圳市格林美高新技术股份有限公司 | Low-oxygen content submicron cobalt powder and cobalt oxalate precursor and manufacturing method thereof |
| CN101745644B (en) * | 2010-03-09 | 2012-04-04 | 南京寒锐钴业有限公司 | Method for preparing cobalt powder |
| JP6350830B2 (en) * | 2015-10-26 | 2018-07-04 | 住友金属鉱山株式会社 | Method for producing seed crystal of cobalt powder |
| CN106346021B (en) * | 2016-09-27 | 2018-08-10 | 南京寒锐钴业股份有限公司 | A kind of method that high pressure hydrogen reduction prepares cobalt powder |
| CN111850632B (en) * | 2020-07-10 | 2022-03-29 | 上海众新五金有限公司 | Activating solution and zinc-nickel electroplating process using same |
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2006
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