CN110976850B - Method for preparing nickel-coated powder by carbonyl vapor deposition - Google Patents

Method for preparing nickel-coated powder by carbonyl vapor deposition Download PDF

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CN110976850B
CN110976850B CN201911244786.0A CN201911244786A CN110976850B CN 110976850 B CN110976850 B CN 110976850B CN 201911244786 A CN201911244786 A CN 201911244786A CN 110976850 B CN110976850 B CN 110976850B
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不公告发明人
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Chengdu Nuclear 857 New Material Co ltd
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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
    • B22F1/17—Metallic particles coated with metal
    • 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
    • B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • B22F9/305—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to a method for preparing nickel-coated powder by carbonyl vapor deposition, which comprises the following steps of firstly, reacting carbon monoxide with active metal nickel under the conditions of normal pressure and 40-100 ℃ to generate carbonyl nickel liquid; then heating the nickel carbonyl liquid to 150-300 ℃, and gasifying the nickel carbonyl liquid into nickel carbonyl gas; mixing nickel carbonyl gas with carrier gas, loading the mixture into a vibration pyrolysis coating furnace, reacting the mixture with a material to be coated in the vibration pyrolysis coating furnace, and thermally decomposing and depositing metal nickel on the surface of the material to be coated by the nickel carbonyl gas to obtain nickel-coated powder; the nickel coating method has high selectivity, and the powder produced by the method has the characteristics of large surface area, high purity, uniform particles, good dispersibility, high chemical reactivity, high activity and the like, and has excellent pressing property and sintering property.

Description

Method for preparing nickel-coated powder by carbonyl vapor deposition
Technical Field
The invention relates to the technical field of nickel-coated powder, and relates to a method for preparing nickel-coated powder by carbonyl vapor deposition.
Background
The carbonyl method is a refining method using a principle of chemical shift reaction. The nickel-coated powder prepared by carbonyl vapor deposition is an ideal method, has high utilization rate of raw materials and good coating effect, but because of CO and generated Ni (CO)4Are all highly toxic substances and Ni (CO)4The volatility of the coating is high, so that the reaction in a sealed system is required, extremely strict anti-toxic measures are required, the requirements on production equipment and processes are high, and the coated powder is required to be coated compactly, uniformly and completely and have stable chemical components.
The main methods for producing nickel-coated powder in the market at present are precipitation-reduction method, chemical nickel plating method, nickel salt decomposition method, hydrothermal pressure hydrogen reduction method and nickel electroplating method.
When the method for producing the nickel-coated powder by adopting the carbonyl vapor deposition method is adopted, the problems that the decomposition rate of the carbonyl nickel is low, the powder coating is incomplete, residual carbonyl nickel liquid exists in the powder, the tail gas has the carbonyl nickel gas which is not decomposed, the product quality is unstable and the like are mainly encountered.
Disclosure of Invention
The invention adopts the method of preparing the nickel-coated powder by carbonyl vapor deposition, adopts the vibration coating decomposing furnace to carry out thermal decomposition coating, ensures that the produced coated powder is uniformly and completely coated, adopts nitrogen and/or carbon monoxide as carrier gas, and ensures that the coated powder is compact and stable in chemical composition by adjusting the temperature and the carrier gas range of the vibration pyrolysis coating furnace without residual nickel carbonyl liquid, thereby having the technical advantages of energy conservation, material conservation and high quality.
The technical scheme adopted by the invention is as follows: the method comprises the following steps:
(1) under the conditions of normal pressure and 40-100 ℃, carbon monoxide reacts with metallic nickel to generate nickel carbonyl liquid;
(2) heating the nickel carbonyl liquid to 150-300 ℃, and gasifying the nickel carbonyl liquid into nickel carbonyl gas;
(3) mixing nickel carbonyl gas with carrier gas, loading the mixed carrier gas into a pyrolysis coating furnace, reacting with a coated material, and thermally decomposing and depositing metal nickel on the surface of the coated material by the nickel carbonyl gas to obtain nickel-coated powder.
Further, the pyrolysis coating furnace in the step 3) is a vibration type pyrolysis coating furnace. The vibration type pyrolysis coating furnace is a pyrolysis coating furnace with a vibration device arranged inside, so that the coated material is vibrated.
Further, the temperature of the nickel carbonyl gas entering the pyrolysis coating furnace in the step 3) is 60-80 ℃.
Further, the temperature in the pyrolysis coating furnace in the step 3) is 200-600 ℃.
Further, the flow rate of the carrier gas in the step 3) is 500 liters to 5000 liters per hour.
Further, the carrier gas in the step 3) comprises at least one of nitrogen and carbon monoxide.
The carbonyl method is a refining method using a principle of chemical shift reaction. For producing high-purity nickel, iron, etc., under the condition of normal pressure and 40-100 deg.C, carbon monoxide can be reacted with active metal nickel to produce a colorless liquid-nickel carbonyl. When the liquid is heated to the temperature of 150-300 ℃, the liquid can be decomposed into nickel and carbon oxide, and the reaction is as follows:
Ni+4CO＝Ni(CO)4 (liquid) Ni (CO)4Ni (solid) +4CO ↓)
The method has high selectivity, and the powder produced by the method has the characteristics of large surface area, high purity, uniform particles, good dispersibility, high chemical reactivity, high activity and the like, and has excellent pressing property and sintering property.
The method for preparing powder by dissociating metal carbonyl compound by carbonyl method, the method uses metal and nonmetal as core material to coat nickel on the surface of the coated material by vapor deposition and reduction method, the principle of the process of coating nickel carbonyl on the surface of the core powder can be expressed as follows:
Figure BDA0002307228050000021
the invention aims to provide a method for preparing nickel-coated powder by carbonyl vapor deposition, which adopts a vibration coating decomposing furnace to carry out thermal decomposition coating to ensure that the produced coated powder is uniformly and completely coated, adopts nitrogen or carbon monoxide as carrier gas, and ensures that the coated powder is compact and stable in chemical composition by adjusting the temperature and the carrier gas range of the vibration pyrolysis coating furnace, has no residual nickel carbonyl liquid, and has the technical advantages of energy conservation, material conservation and high quality.
Aiming at the problems that the decomposition rate of nickel carbonyl is low, nickel carbonyl liquid remains in powder and chemical components of a product are unstable in the coating process, the thermal decomposition rate of the nickel carbonyl liquid is improved by adjusting the thermal decomposition temperature range, and the chemical components of the product are stable; the residual nickel carbonyl liquid in the powder is solved by adopting nitrogen or carbon monoxide as carrier gas, and the nickel carbonyl gas in the tail gas is reduced; through the technical scheme, the produced nickel-coated powder is compact, uniform and complete in coating and stable in chemical components, and meets the technical requirements and the use requirements of products.
The scheme adopts a vibration coating decomposing furnace for thermal decomposition coating, so that the produced coating powder is uniformly and completely coated, adopts nitrogen or carbon monoxide as carrier gas, and adjusts the temperature of the decomposing furnace and the range of the carrier gas to ensure that the coated powder is compact and stable in chemical composition without residual nickel carbonyl liquid.
The invention has the beneficial effects that:
the nickel coating method has high selectivity, and the powder produced by the method has the characteristics of large surface area, high purity, uniform particles, good dispersibility, high chemical reactivity, high activity and the like, and has excellent pressing property and sintering property.
Drawings
FIG. 1 is a flow chart of the apparatus of the present invention;
FIG. 2 is a process flow diagram of the present invention.
Detailed Description
In order to further illustrate the technical effects of the present invention, the present invention is specifically described below by way of examples.
Example 1
A method for preparing nickel-coated powder by carbonyl vapor deposition, which is applied to a nickel-coating process, comprises the following steps:
1) the preparation step, the material to be coated is placed in a vibration pyrolysis coating furnace, the material to be coated is a material to be coated, the material to be coated can be a metal or nonmetal material, carbon monoxide and metallic nickel are prepared under the conditions of normal pressure and 40 ℃, and then the prepared nickel carbonyl liquid is stored in a liquid storage tank for later use;
2) putting the nickel carbonyl liquid prepared in the step (1) into an evaporator, heating the nickel carbonyl liquid to 150 ℃ by a heating device, gasifying the nickel carbonyl liquid into nickel carbonyl gas, and putting carrier gas into the evaporator;
3) the carrier gas and the nickel carbonyl gas enter the vibration pyrolysis coating furnace from the evaporator, the temperature of the nickel carbonyl gas entering the vibration pyrolysis coating furnace is 60 ℃, the flow rate of the carrier gas is 500 liters/hour, the vibration pyrolysis coating furnace is heated to 200 ℃ by a heating device, the nickel carbonyl gas and the coated material undergo vapor deposition reaction at high temperature, the metal nickel is coated on the surface of the coated material after the nickel carbonyl gas is thermally decomposed, the carbon monoxide, the carrier gas and the unreacted nickel carbonyl gas are discharged into a tail gas recovery device from a buffer, and the carrier gas is carbon monoxide;
4) screening qualified products from the coated material prepared in the vibration pyrolysis coating furnace, and packaging the qualified products into finished products for storage after inspection.
The nickel-coated powder prepared by the embodiment has high coating integrity, no residual nickel carbonyl liquid in the powder, low content of undecomposed nickel carbonyl gas in tail gas and stable product quality.
Example 2
A method for preparing nickel-coated powder by carbonyl vapor deposition, which is applied to a nickel-coating process, comprises the following steps:
1) the preparation step, the material to be coated is placed in a vibration pyrolysis coating furnace, the material to be coated is a material to be coated, the material to be coated can be a metal or nonmetal material, carbon monoxide and metallic nickel are prepared under the conditions of normal pressure and 100 ℃, and then the prepared nickel carbonyl liquid is stored in a liquid storage tank for later use;
2) putting the nickel carbonyl liquid prepared in the step (1) into an evaporator, heating the nickel carbonyl liquid to 300 ℃ by a heating device, gasifying the nickel carbonyl liquid into nickel carbonyl gas, and putting carrier gas into the evaporator;
3) the carrier gas and the nickel carbonyl gas enter the vibration pyrolysis coating furnace from the evaporator, the temperature of the nickel carbonyl gas entering the vibration pyrolysis coating furnace is 80 ℃, the flow rate of the carrier gas is 5000 liters/hour, the vibration pyrolysis coating furnace is heated to 600 ℃ by a heating device, the nickel carbonyl gas and the coated material undergo vapor deposition reaction at high temperature, the metal nickel is coated on the surface of the coated material after the nickel carbonyl gas is thermally decomposed, the carbon monoxide, the carrier gas and the unreacted nickel carbonyl gas are discharged into a tail gas recovery device from a buffer, and the carrier gas is carbon monoxide;
4) screening qualified products from the coated material prepared in the vibration pyrolysis coating furnace, and packaging the qualified products into finished products for storage after inspection.
The nickel-coated powder prepared by the embodiment has high coating integrity, no residual nickel carbonyl liquid in the powder, low content of undecomposed nickel carbonyl gas in tail gas and stable product quality.
Example 3
A method for preparing nickel-coated powder by carbonyl vapor deposition, which is applied to a nickel-coating process, comprises the following steps:
1) the preparation step, the material to be coated is placed in a vibration pyrolysis coating furnace, the material to be coated is a material to be coated, the material to be coated can be a metal or nonmetal material, carbon monoxide and metallic nickel are prepared under the conditions of normal pressure and 70 ℃, and then the prepared nickel carbonyl liquid is stored in a liquid storage tank for later use;
2) putting the nickel carbonyl liquid prepared in the step (1) into an evaporator, heating the nickel carbonyl liquid to 225 ℃ by a heating device, gasifying the nickel carbonyl liquid into nickel carbonyl gas, and putting carrier gas into the evaporator;
3) the carrier gas and the nickel carbonyl gas enter the vibration pyrolysis coating furnace from the evaporator, the temperature of the nickel carbonyl gas entering the vibration pyrolysis coating furnace is 70 ℃, the flow rate of the carrier gas is 2750 liters/hour, the vibration pyrolysis coating furnace is heated to 400 ℃ by a heating device, the nickel carbonyl gas and the coated material undergo vapor deposition reaction at high temperature, the metal nickel is coated on the surface of the coated material after the nickel carbonyl gas is thermally decomposed, the carbon monoxide, the carrier gas and the unreacted nickel carbonyl gas are discharged into a tail gas recovery device from a buffer, and the carrier gas is carbon monoxide;
4) screening qualified products from the coated material prepared in the vibration pyrolysis coating furnace, and packaging the qualified products into finished products for storage after inspection.
The nickel-coated powder prepared by the embodiment has high coating integrity, no residual nickel carbonyl liquid in the powder, low content of undecomposed nickel carbonyl gas in tail gas and stable product quality.
Example 4
A method for preparing nickel-coated powder by carbonyl vapor deposition, which is applied to a nickel-coating process, comprises the following steps:
1) the preparation step, the material to be coated is placed in a vibration pyrolysis coating furnace, the material to be coated is a material to be coated, the material to be coated can be a metal or nonmetal material, carbon monoxide and metallic nickel are prepared under the conditions of normal pressure and 50 ℃, and then the prepared nickel carbonyl liquid is stored in a liquid storage tank for later use;
2) putting the nickel carbonyl liquid prepared in the step (1) into an evaporator, heating the nickel carbonyl liquid to 180 ℃ by a heating device, gasifying the nickel carbonyl liquid into nickel carbonyl gas, and putting carrier gas into the evaporator;
3) the carrier gas and the nickel carbonyl gas enter the vibration pyrolysis coating furnace from the evaporator, the temperature of the nickel carbonyl gas entering the vibration pyrolysis coating furnace is 65 ℃, the flow rate of the carrier gas is 1000 liters/hour, the vibration pyrolysis coating furnace is heated to 300 ℃ by a heating device, the nickel carbonyl gas and the coated material undergo vapor deposition reaction at high temperature, the metal nickel is coated on the surface of the coated material after the nickel carbonyl gas is thermally decomposed, the carbon monoxide, the carrier gas and the unreacted nickel carbonyl gas are discharged into a tail gas recovery device from a buffer, and the carrier gas is carbon monoxide;
4) screening qualified products from the coated material prepared in the vibration pyrolysis coating furnace, and packaging the qualified products into finished products for storage after inspection.
The nickel-coated powder prepared by the embodiment has high coating integrity, no residual nickel carbonyl liquid in the powder, low content of undecomposed nickel carbonyl gas in tail gas and stable product quality.
Example 5
A method for preparing nickel-coated powder by carbonyl vapor deposition, which is applied to a nickel-coating process, comprises the following steps:
1) the preparation step, the material to be coated is placed in a vibration pyrolysis coating furnace, the material to be coated is a material to be coated, the material to be coated can be a metal or nonmetal material, carbon monoxide and metallic nickel are prepared under the conditions of normal pressure and 80 ℃, and then the prepared nickel carbonyl liquid is stored in a liquid storage tank for later use;
2) putting the nickel carbonyl liquid prepared in the step (1) into an evaporator, heating the nickel carbonyl liquid to 270 ℃ by a heating device, gasifying the nickel carbonyl liquid into nickel carbonyl gas, and putting carrier gas into the evaporator;
3) the carrier gas and the nickel carbonyl gas enter the vibration pyrolysis coating furnace from the evaporator, the temperature of the nickel carbonyl gas entering the vibration pyrolysis coating furnace is 75 ℃, the flow rate of the carrier gas is 3500L/h, the vibration pyrolysis coating furnace is heated to 500 ℃ by a heating device, the nickel carbonyl gas and the coated material undergo vapor deposition reaction at high temperature, the metal nickel is coated on the surface of the coated material after the nickel carbonyl gas is thermally decomposed, the carbon monoxide, the carrier gas and the unreacted nickel carbonyl gas are discharged into a tail gas recovery device from a buffer, and the carrier gas is carbon monoxide;
4) screening qualified products from the coated material prepared in the vibration pyrolysis coating furnace, and packaging the qualified products into finished products for storage after inspection.
The nickel-coated powder prepared by the embodiment has high coating integrity, no residual nickel carbonyl liquid in the powder, low content of undecomposed nickel carbonyl gas in tail gas and stable product quality.
Comparative example 1
A method for preparing nickel-coated powder by carbonyl vapor deposition, which is applied to a nickel-coating process, comprises the following steps:
1) the preparation step, the material to be coated is placed in a vibration pyrolysis coating furnace, the material to be coated is a material to be coated, the material to be coated can be a metal or nonmetal material, carbon monoxide and metallic nickel are prepared under the conditions of normal pressure and 70 ℃, and then the prepared nickel carbonyl liquid is stored in a liquid storage tank for later use;
2) putting the nickel carbonyl liquid prepared in the step (1) into an evaporator, heating the nickel carbonyl liquid to 225 ℃ by a heating device, gasifying the nickel carbonyl liquid into nickel carbonyl gas, and putting carrier gas into the evaporator;
3) the carrier gas and the nickel carbonyl gas enter the vibration pyrolysis coating furnace from the evaporator, the temperature of the nickel carbonyl gas entering the vibration pyrolysis coating furnace is 70 ℃, the flow rate of the carrier gas is 2750 liters/hour, the vibration pyrolysis coating furnace is heated to 400 ℃ by a heating device, the nickel carbonyl gas and the coated material undergo vapor deposition reaction at high temperature, the metal nickel is coated on the surface of the coated material after the nickel carbonyl gas is thermally decomposed, the carbon monoxide, the carrier gas and the unreacted nickel carbonyl gas are discharged into a tail gas recovery device from a buffer, and the carrier gas is nitrogen;
4) screening qualified products from the coated material prepared in the vibration pyrolysis coating furnace, and packaging the qualified products into finished products for storage after inspection.
The nickel-coated powder prepared by the comparative example has incomplete coating, residual nickel carbonyl liquid in the powder, undecomposed nickel carbonyl gas in tail gas and unstable product quality.
Comparative example 2
A method for preparing nickel-coated powder by carbonyl vapor deposition, which is applied to a nickel-coating process, comprises the following steps:
1) the preparation step, the material to be coated is placed in a vibration pyrolysis coating furnace, the material to be coated is a material to be coated, the material to be coated can be a metal or nonmetal material, carbon monoxide and metallic nickel are prepared under the conditions of normal pressure and 70 ℃, and then the prepared nickel carbonyl liquid is stored in a liquid storage tank for later use;
2) putting the nickel carbonyl liquid prepared in the step (1) into an evaporator, heating the nickel carbonyl liquid to 225 ℃ by a heating device, gasifying the nickel carbonyl liquid into nickel carbonyl gas, and putting carrier gas into the evaporator;
3) the carrier gas and the nickel carbonyl gas enter the vibration pyrolysis coating furnace from the evaporator, the temperature of the nickel carbonyl gas entering the vibration pyrolysis coating furnace is 70 ℃, the flow rate of the carrier gas is 2750 liters/hour, the vibration pyrolysis coating furnace is heated to 400 ℃ by a heating device, the nickel carbonyl gas and the coated material undergo vapor deposition reaction at high temperature, the metal nickel is coated on the surface of the coated material after the nickel carbonyl gas is thermally decomposed, the carbon monoxide, the carrier gas and the unreacted nickel carbonyl gas are discharged into a tail gas recovery device from a buffer, and the carrier gas is carbon monoxide;
4) screening qualified products from the coated material prepared in the vibration pyrolysis coating furnace, and packaging the qualified products into finished products for storage after inspection.
The nickel-coated powder prepared by the comparative example has incomplete coating, residual nickel carbonyl liquid in the powder, undecomposed nickel carbonyl gas in tail gas and unstable product quality.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and although the technical solutions of the present invention are described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the present invention, which should be covered by the protection scope of the present invention.

Claims (6)

1. The method for preparing the nickel-coated powder by carbonyl vapor deposition is characterized by comprising the following steps of:
1) under the conditions of normal pressure and 40-100 ℃, carbon monoxide reacts with metallic nickel to generate nickel carbonyl liquid;
2) heating the nickel carbonyl liquid to the temperature of 150 ℃ and 300 ℃, and gasifying the nickel carbonyl liquid into nickel carbonyl gas;
3) mixing nickel carbonyl gas with carrier gas, loading the mixed carrier gas into a pyrolysis coating furnace, reacting with a coated material, and thermally decomposing and depositing metal nickel on the surface of the coated material by the nickel carbonyl gas to obtain nickel-coated powder.
2. The method for preparing nickel-coated powder by carbonyl vapor deposition according to claim 1, wherein the pyrolysis coating furnace in step 3) is a vibrating pyrolysis coating furnace.
3. The method for preparing nickel-coated powder by carbonyl vapor deposition according to claim 1, wherein the temperature of the nickel carbonyl gas entering the pyrolysis coating furnace in the step 3) is 60 ℃ to 80 ℃.
4. The method for preparing nickel-coated powder using carbonyl vapor deposition according to claim 1, wherein the temperature in the pyrolysis coating furnace in step 3) is 200 ℃ to 600 ℃.
5. The method for preparing nickel-coated powder using carbonyl vapor deposition as claimed in claim 1, wherein the flow rate of the carrier gas in step 3) is 500 l/hr to 5000 l/hr.
6. The method of claim 1, wherein the carrier gas in step 3) comprises at least one of nitrogen and carbon monoxide.
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JPH0459903A (en) * 1990-06-28 1992-02-26 Tdk Corp Manufacture of ferromagnetic super fine particles, ferromagnetic super fine particles for fixing physiologically active material and physiologically active material fixing ferromagnetic super fine particles
CN100463749C (en) * 2006-11-24 2009-02-25 金川集团有限公司 Method for producing compounding powder by using thermal decomposition of carbonyl nickel in vibration fluidized layer
CN102888593B (en) * 2011-07-20 2014-07-02 航天材料及工艺研究所 Device for coating pyrolytic carbon on graphite sphere surface and gas-phase carbon depositing method
CN102717067A (en) * 2012-06-05 2012-10-10 金川集团股份有限公司 Method for preparing nickel-coated powder
CN203144511U (en) * 2013-03-15 2013-08-21 金川集团股份有限公司 Pyrolysis furnace for preparing nickel rod by chemical vapour deposition method
CN106001549B (en) * 2016-05-11 2018-02-06 江油核宝纳米材料有限公司 The preparation method of carbonyl process nickel bag graphite

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