CN100497729C - Method for preparing carbon coating cobalt nano particle by cobalt/aluminum catalytic chemical gaseous phase deposition - Google Patents
Method for preparing carbon coating cobalt nano particle by cobalt/aluminum catalytic chemical gaseous phase deposition Download PDFInfo
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- CN100497729C CN100497729C CNB2007100586253A CN200710058625A CN100497729C CN 100497729 C CN100497729 C CN 100497729C CN B2007100586253 A CNB2007100586253 A CN B2007100586253A CN 200710058625 A CN200710058625 A CN 200710058625A CN 100497729 C CN100497729 C CN 100497729C
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- 239000010941 cobalt Substances 0.000 title claims abstract description 50
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 50
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 50
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910052782 aluminium Inorganic materials 0.000 title claims description 38
- 239000011248 coating agent Substances 0.000 title claims description 31
- 238000000576 coating method Methods 0.000 title claims description 31
- 230000008021 deposition Effects 0.000 title claims description 6
- 239000000126 substance Substances 0.000 title claims description 6
- 230000003197 catalytic effect Effects 0.000 title claims description 5
- 239000007792 gaseous phase Substances 0.000 title claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012018 catalyst precursor Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 36
- 239000004411 aluminium Substances 0.000 claims description 33
- 239000002131 composite material Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 238000004523 catalytic cracking Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000012716 precipitator Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229940045029 cobaltous nitrate hexahydrate Drugs 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 238000004050 hot filament vapor deposition Methods 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 2
- 241000234282 Allium Species 0.000 description 1
- 235000002732 Allium cepa var. cepa Nutrition 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention relates to a method for preparing carbon-coated cobalt nanoparticles by Co/Al catalytic chemical vapor deposition, belonging to the technical field of preparation of carbon-coated cobalt nanoparticles. The method comprises: preparing Co/Al catalyst precursor (CoO/Al) from cobaltous nitrate hexahydrate and aluminum powder as raw materials at a given mass ratio by deposition-precipitation method; and allowing the reactions of nitrogen gas or hydrogen gas and methane in a reactor in the presence of CoO/Al at a given temperature by chemical vapor deposition. The invention has the advantages that the cobalt content of Co/Al catalyst is accurately determined during the preparation process, so as to control the yield of carbon-coated cobalt nanoparticles; the reaction parameters of chemical vapor deposition are adjusted to control the shape and size of carbon-coated cobalt nanoparticles. Therefore, the obtained carbon-coated cobalt nanoparticles have high purity, good dispersibility and uniform size.
Description
Technical field
The present invention relates to a kind of method for preparing carbon coating cobalt nano-particle/aluminium composite powder with cobalt/aluminum catalytic chemical gaseous phase deposition.Belong to carbon coating cobalt nano-particle/aluminium composite powder technology of preparing.
Background technology
Carbon coating cobalt nano-particle is a kind of novel nano carbon/cobalt composite material, and wherein the multilayer graphite flake layer closely forms class onion structure around the cobalt nano-particle ordered arrangement, and cobalt nanometer particle is in the core of carbon coating layer.Carbon coating cobalt nano-particle has been avoided the influence of environment to cobalt nano-particle, the stability that has kept cobalt nano-particle, improve the biocompatibility of cobalt nano-particle, can be used as electric wave shielding material, magnetic recording material, cell negative electrode material, nuclear waste disposal material, fine ceramics material and anti-biotic material etc.At present, the method for preparing carbon coating cobalt nano-particle mainly contains arc discharge method, pyrolysis method, liquid impregnation method and explosion method etc., but aforesaid method exists in the process of preparation carbon coating cobalt nano-particle problems such as temperature required height, energy are big, complex process, poor controllability.
Summary of the invention
The present invention aims to provide and a kind ofly prepares the method for carbon coating cobalt nano-particle/aluminium composite powder with cobalt/aluminum catalytic chemical gaseous phase deposition, and this procedure is simple, and prepared carbon coating cobalt nano-particle purity height, good dispersity, particle size are even.
The present invention is realized by the following technical programs: a kind of preparation method with cobalt/al catalyst chemical gas phase deposition carbon coating cobalt nano-particle/aluminium composite powder, it is characterized in that comprising following process,
1) deposition-precipitator method prepare the Co/Al catalyst precursor
Is (0.05-1.23) with cobalt nitrate hexahydrate and aluminium powder in mass ratio: 1 ratio joins in the deionized water, being mixed with concentration is the cobalt nitrate hexahydrate solution that 0.01-1mol/L contains aluminium powder, dropping sodium or ammoniacal liquor make solution be neutral and are precipitated in solution, and making the Co/Al mass ratio is (0.01-0.25): 1 Co (OH)
2/ Al binary colloidal; With this Co (OH)
2/ Al binary colloidal dewaters under 150 ℃-300 ℃, nitrogen atmosphere, and at 350 ℃ of-500 ℃ of temperature lower calcinations, obtains Co/Al catalyst precursor CoO/Al.
2) chemical Vapor deposition process prepares carbon coating cobalt nano-particle/aluminium composite powder
The Co/Al catalyst precursor powder that step 1) is made is layered in the quartz boat, quartz boat is placed the reactor flat-temperature zone again; Feed the nitrogen replacement air, reactor is warming up to 400 ℃-650 ℃ then, and feed hydrogen to reactor with 25-400ml/min, and kept 0.5-6 hour, close hydrogen afterwards, with volume ratio is (1-12): 1 the nitrogen and the gas mixture of methane, or be (1-12): 1 the hydrogen and the gas mixture of methane with volume ratio, it or is (1-12): the gas mixture of 1 nitrogen and hydrogen and methane with volume ratio, feed reactor with the 120-780ml/min gas mixture, carry out catalytic cracking reaction 0.1h-6h under 400 ℃-650 ℃, reactor is chilled to room temperature under nitrogen atmosphere afterwards, and making particle diameter is carbon coating cobalt nano-particle/aluminium composite powder of 25-70nm.
The present invention has the following advantages: the Co/Al catalyzer that is adopted can carry out accurately determining in preparation process, thereby can be controlled the productive rate of carbon coating cobalt nano-particle/aluminium composite powder cobalt contents; In chemical vapor deposition processes by reaction parameter is regulated, thereby can realize control to carbon coating cobalt nano-particle form and size, therefore, adopt the present invention to prepare carbon coating cobalt nano-particle/aluminium composite powder and have characteristics such as product purity height, good dispersity, size be even.In addition, technological process of the present invention is simple.
Description of drawings
Fig. 1 is the TEM figure of example 2 prepared carbon coating cobalt nano-particle/aluminium composite powders of the present invention.
Fig. 2 is the HRTEM figure of example 2 prepared carbon coating cobalt nano-particles of the present invention.
Central black zone shown among the figure is a cobalt nano-particle, and the layer-shaped area that its outside coats is a carbon-coating.
Embodiment
Describe the present invention in detail below in conjunction with embodiment, these embodiment only are used to illustrate the present invention, do not limit the present invention.
Use raw material: cobalt nitrate hexahydrate, commercially available, purity〉96%; Aluminium powder, commercially available, 400 orders.
Embodiment 1
Is that the ratio of 0.05:1 joins in the deionized water with cobalt nitrate hexahydrate and aluminium powder in mass ratio, being mixed with concentration is the cobalt nitrate hexahydrate solution that 0.01mol/L contains aluminium powder, dropping sodium makes solution be neutral and is precipitated in solution, makes the Co that the Co/Al mass ratio is 0.01:1 (OH)
2/ Al binary colloidal; This binary colloidal is dewatered under 240 ℃, nitrogen atmosphere, and, obtain Co/Al catalyst precursor CoO/Al at 400 ℃ of temperature lower calcinations; The Co/Al catalyst precursor powder of gained is layered in the quartz boat, again quartz boat is placed the reactor flat-temperature zone; Feed the air in the nitrogen replacement pipe, reactor is warming up to 600 ℃ then, and feed hydrogen to reactor with 200ml/min, and kept 2 hours, closing hydrogen afterwards, is that the nitrogen of 7:1 and the gas mixture of methane feed reactor with 480ml/min with volume ratio, carries out catalytic cracking reaction 0.5h under 600 ℃, reactor is chilled to room temperature under nitrogen atmosphere afterwards, makes productive rate and be 0.08%, median size is carbon coating cobalt particle/aluminium composite powder of 30nm.
Embodiment 2
The experiment condition of present embodiment and process are with embodiment 1, and difference is that the catalytic cracking reaction time is 1h, make productive rate and be 0.2%, median size is carbon coating cobalt particle/aluminium composite powder of 36nm.
Embodiment 3
The experiment condition of present embodiment and process are with embodiment 1, and difference is that the catalytic cracking reaction time is 2h, make productive rate and be 0.35%, median size is carbon coating cobalt particle/aluminium composite powder of 45nm.
Embodiment 4
Is that the ratio of 0.55:1 joins in the deionized water with cobalt nitrate hexahydrate and aluminium powder in mass ratio, being mixed with concentration is the cobalt nitrate hexahydrate solution that 0.1mol/L contains aluminium powder, dropping sodium makes solution be neutral and is precipitated in solution, makes the Co that the Co/Al mass ratio is 0.11:1 (OH)
2/ Al binary colloidal; Following steps are identical with embodiment 1 with condition, make productive rate and be 0.9%, median size is carbon coating cobalt particle/aluminium composite powder of 35nm.
Embodiment 5
The experiment condition of present embodiment and process are with embodiment 4, and difference is that the catalytic cracking reaction time is 1h, make productive rate and be 1.6%, median size is carbon coating cobalt particle/aluminium composite powder of 42nm.
Embodiment 6
The experiment condition of present embodiment and process are with embodiment 4, and difference is that the catalytic cracking reaction time is 2h, make productive rate and be 3%, median size is carbon coating cobalt particle/aluminium composite powder of 50nm.
Embodiment 7
Is that the ratio of 1.23:1 joins in the deionized water with cobalt nitrate hexahydrate and aluminium powder in mass ratio, being mixed with concentration is the cobalt nitrate hexahydrate solution that 1mol/L contains aluminium powder, dropping sodium makes solution be neutral and is precipitated in solution, makes the Co that the Co/Al mass ratio is 0.25:1 (OH)
2/ Al binary colloidal; Following steps are identical with embodiment 1 with condition, and difference is that the catalytic cracking reaction time is 1h, make productive rate and be 2.8%, median size is carbon coating cobalt particle/aluminium composite powder of 52nm.
Embodiment 8
The experiment condition of present embodiment and process are with embodiment 7, and difference is that the catalytic cracking reaction time is 2h, make productive rate and be 5.4%, median size is carbon coating cobalt particle/aluminium composite powder of 61nm.
Embodiment 9
The experiment condition of present embodiment and process are with embodiment 1, and it is the hydrogen of 7:1 and the gas mixture of methane that difference is to adopt volume ratio, make productive rate and be 0.07%, median size is carbon coating cobalt particle/aluminium composite powder of 27nm.
Claims (1)
1, a kind of preparation method with cobalt/aluminum catalytic chemical gaseous phase deposition carbon coating cobalt nano-particle/aluminium composite powder is characterized in that comprising following process,
1) deposition-precipitator method prepare the Co/Al catalyst precursor
Is (0.05-1.23) with cobalt nitrate hexahydrate and aluminium powder in mass ratio: 1 ratio joins in the deionized water, being mixed with concentration is the cobalt nitrate hexahydrate solution that 0.01-1mol/L contains aluminium powder, dropping sodium or ammoniacal liquor make solution be neutral and are precipitated in solution, and making the Co/Al mass ratio is (0.01-0.25): 1 Co (OH)
2/ Al binary colloidal; With this Co (OH)
2/ Al binary colloidal dewaters under 150 ℃-300 ℃, nitrogen atmosphere, and at 350 ℃ of-500 ℃ of temperature lower calcinations, obtains Co/Al catalyst precursor CoO/Al;
2) chemical Vapor deposition process prepares carbon coating cobalt nano-particle/aluminium composite powder
The Co/Al catalyst precursor powder that step 1) is made is layered in the quartz boat, quartz boat is placed the reactor flat-temperature zone again; Feed the nitrogen replacement air, reactor is warming up to 400 ℃-650 ℃ then, and feed hydrogen to reactor with 25-400ml/min, and kept 0.5-6 hour, close hydrogen afterwards, with volume ratio is (1-12): 1 the nitrogen and the gas mixture of methane, or be (1-12): 1 the hydrogen and the gas mixture of methane with volume ratio, it or is (1-12): the gas mixture of 1 nitrogen and hydrogen and methane with volume ratio, feed reactor with the 120-780ml/min gas mixture, carry out catalytic cracking reaction 0.1h-6h under 400 ℃-650 ℃, reactor is chilled to room temperature under nitrogen atmosphere afterwards, and making particle diameter is carbon coating cobalt nano-particle/aluminium composite powder of 25-70nm.
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| CNB2007100586253A CN100497729C (en) | 2007-08-08 | 2007-08-08 | Method for preparing carbon coating cobalt nano particle by cobalt/aluminum catalytic chemical gaseous phase deposition |
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| CNB2007100586253A CN100497729C (en) | 2007-08-08 | 2007-08-08 | Method for preparing carbon coating cobalt nano particle by cobalt/aluminum catalytic chemical gaseous phase deposition |
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| CN103695864B (en) * | 2014-01-06 | 2016-05-11 | 河北工业大学 | The preparation method of carbon coating cobalt metal nanoparticle |
| CN107824785B (en) * | 2017-09-29 | 2019-06-04 | 中国航发北京航空材料研究院 | A kind of low laser reflectivity powder particle and preparation method |
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Non-Patent Citations (4)
| Title |
|---|
| CVD法制备的碳包覆（Fe，Co）纳米粒子的结构及电磁特性. 雷中兴等.磁性材料及器件，第34卷第4期. 2003 |
| CVD法制备的碳包覆（Fe，Co）纳米粒子的结构及电磁特性. 雷中兴等.磁性材料及器件，第34卷第4期. 2003 * |
| Large-scale preparation of carbon-encapsulated cobaltnanoparticles by the catalytic method. B.H.Liu et al.Chemical Physics Letters. 2002 |
| Large-scale preparation of carbon-encapsulated cobaltnanoparticles by the catalytic method. B.H.Liu et al.Chemical Physics Letters. 2002 * |
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