CN111774579A - Al/Ni composite particle and preparation method thereof - Google Patents

Al/Ni composite particle and preparation method thereof Download PDF

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CN111774579A
CN111774579A CN201910271798.6A CN201910271798A CN111774579A CN 111774579 A CN111774579 A CN 111774579A CN 201910271798 A CN201910271798 A CN 201910271798A CN 111774579 A CN111774579 A CN 111774579A
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aluminum powder
composite particles
nickel
sodium hydroxide
suspension
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CN111774579B (en
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韩志伟
李亚宁
王伯良
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Nanjing University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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

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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a preparation method of Al/Ni composite particles. The method specifically comprises the following steps: mixing nano or micron aluminum powder, nickel salt and ethanol to form a suspension, and mixing sodium hydroxide and ethanol to form a transparent solution; under the conditions of required environmental temperature and pH value, dropwise adding a sodium hydroxide solution into the suspension, reacting the sodium hydroxide with aluminum oxide on the surface of the aluminum powder to expose an aluminum core in the aluminum powder, then performing a displacement reaction on the exposed aluminum core and nickel ions, depositing nano nickel particles generated by the reaction on the surface of the aluminum powder, and finally obtaining the Al/Ni composite particles with the core-shell structure through suction filtration and vacuum drying. The preparation method has the advantages of small environmental pollution, simple process and low cost in the preparation process.

Description

Al/Ni composite particle and preparation method thereof
Technical Field
The invention belongs to the technical field of micro-nano energetic materials, and provides an Al/Ni composite particle and a preparation method thereof.
Background
The micro-nano aluminum powder is one of the most commonly used high-activity metal powders in the field of current energetic materials, and has extremely important significance for developing and researching high-performance weapon ammunition. The small-particle aluminum powder, especially for nano aluminum powder, is easy to react with oxygen, water and the likeShould, a compact and chemically stable compound Al be formed2O3The reaction of the residual active aluminum and the oxidant is hindered, and the energy release efficiency is greatly limited; meanwhile, the aluminum powder is often agglomerated and sintered during combustion to generate larger particles, so that the activity of the aluminum powder is reduced and the reaction is incomplete. For example, for aluminum powder particles having an average particle diameter of 80nm, the active aluminum content is only about 75%, and chemically inert Al is used2O3The mass ratio is extremely high, the average size of the aggregate and the sintered body can reach 3-6 μm, so that the advantages of the nano effect of the aluminum powder are lost, and the characteristics of high reactivity, high reaction rate and the like cannot be exerted to the maximum extent.
Researches find that the nano nickel particles as a coating material of the aluminum powder have various advantages for improving the reaction characteristics of the aluminum powder. Firstly, compared with aluminum, nickel has lower reactivity in a natural state and is not easy to chemically react with oxygen or water, so that the nickel coating layer with a certain thickness is used for replacing aluminum oxide on the surface of aluminum powder, the oxidation of the aluminum powder core can be prevented to a great extent, and the dispersibility of the nano aluminum powder is improved; secondly, nickel also undergoes redox reaction under certain conditions, and Al is replaced by nickel2O3So that the aluminum powder system is made of Al/Al2O3Change to Al/Ni/Al2O3The total active substance content of the system is improved; in addition, another literature reports that the ignition performance and the combustion performance of the nano aluminum powder can be improved by coating nickel on the surface of the aluminum powder, and the energy release efficiency of the nano aluminum powder is further improved.
At present, a method for preparing nickel-coated aluminum powder mainly comprises a vapor deposition method and a chemical plating method, and patent CN201210180759.3 (application date, 6/5/2012 and publication date, 2012, 10/10) discloses a method for preparing nickel-coated micron aluminum powder by a vapor deposition method, aluminum powder particles form a counter flow with nickel carbonyl steam/carbon monoxide mixed gas sprayed from a nozzle at the lower side of a fluidized bed reactor in the fluidized bed reactor, in the counter flow process, the nickel carbonyl gas is thermally decomposed on the surface of the aluminum powder to generate metal nickel, and the metal nickel is deposited on the surface of the aluminum powder, so that the micron aluminum powder is coated. TheThe method has complex technological parameters, the preparation process is not under the conditions of normal temperature and normal pressure, certain potential safety hazard exists, the equipment cost is high, and strict requirements are provided for various performances of the equipment. Patent CN201310359074.X (application date 8/16/2013, publication date 12/11/2013) describes a method for preparing nickel-coated aluminum micropowder by electroless plating, which comprises the steps of performing alkaline washing on aluminum powder with NaOH aqueous solution, adding the alkaline washed aluminum powder into a first main salt solution consisting of nickel sulfate and citric acid, adding a surfactant, and then dropwise adding NH into the plating solution at a constant speed4And F, initiating a displacement reaction by using a solution F, finally retreating the plating solution by using a second main salt solution, a sodium hypophosphite solution, ammonia water, an ammonium sulfate solution and the like, performing suction filtration, then alternately cleaning with water and absolute ethyl alcohol for multiple times, and then performing vacuum drying to obtain a final product. The method has a complex process flow, aluminum powder is coated and nickel-plated in two steps, more chemical waste liquid is left in each nickel plating process, so that raw materials are wasted, more ammonia water is used in the final treatment, and the environment is seriously polluted; in addition, the whole nickel plating process adopts an aqueous solution environment, and the oxidation reduction reaction of the aluminum powder and water is not considered, so that a large amount of active aluminum is lost. Patent CN200710056768.0 (application date 2/9/2008/8/13) discloses a method for nickel coating on nano aluminum powder, which comprises adding nano aluminum powder into glycol dimethyl ether liquid, and stirring to disperse the nano aluminum powder uniformly; adding nickel acetylacetonate into glycol dimethyl ether liquid, and stirring to completely dissolve the nickel acetylacetonate into the glycol dimethyl ether liquid to form uniformly mixed liquid; mixing the two liquids to ensure that the nickel acetylacetonate is spontaneously adsorbed on the nano aluminum powder in the glycol dimethyl ether liquid; and naturally volatilizing and drying the adsorbed nano aluminum powder, and taking out to obtain the nickel-coated nano aluminum powder with the core-shell structure. The method uses the organic solvent with stronger volatility in the whole process, all the organic solvents are finally volatilized and discharged into the atmospheric environment to obtain the final product, so that the environmental pollution is caused, meanwhile, the use of a large amount of organic solvents also causes higher preparation cost, and in addition, the glycol dimethyl ether has the characteristics of flammability and explosiveness and stronger toxicity, so that the probability of dangerous accidents in the sample preparation process is increased.
In conclusion of research on the preparation method of the nickel-coated micro-nano aluminum powder, the existing preparation method is not simple, convenient, green and safe, has high economic cost and is not suitable for large-scale application and production to prepare Al/Ni composite particles.
Disclosure of Invention
The invention aims to provide Al/Ni composite particles and a preparation method thereof, which are used for preventing aluminum powder from being oxidized and inactivated in air, reducing ignition delay of the aluminum powder, improving the combustion reaction rate of the aluminum powder and solving the problems of incomplete energy release of the aluminum powder and the like.
The technical scheme for realizing the purpose of the invention is as follows:
an Al/Ni composite particle comprises 3.6-14.8% by mass of nickel, 68.7-96.0% by mass of activated aluminum and 0.4-16.5% by mass of alumina.
Furthermore, the composite particles are of a core-shell structure, the nano aluminum powder is a core, and the nickel is coated on the surface of the nano aluminum powder.
The preparation method of the Al/Ni composite particle comprises the following steps: (1) weighing sodium hydroxide, and adding the sodium hydroxide into absolute ethyl alcohol to form a transparent solution; (2) weighing aluminum powder and nickel salt, adding the aluminum powder and nickel salt into absolute ethyl alcohol, and then carrying out ultrasonic dispersion for 30min to form uniform suspension; (3) transferring the transparent solution and the suspension prepared in the steps (1) and (2) into a constant-temperature water bath kettle, setting the water bath temperature to be 35-45 ℃, and enabling the temperatures of the transparent solution and the suspension to reach the set temperature; (4) dropwise adding the transparent solution prepared in the step (1) into the suspension prepared in the step (2), and violently stirring the suspension in the dropwise adding process, wherein the total reaction time is controlled to be 5-10 min; (5) and after the reaction is finished, carrying out suction filtration and vacuum drying, and collecting the composite particles.
Compared with the prior art, the invention has the following remarkable advantages: the Al/Ni composite particles have good corrosion resistance in natural environment, and can keep the content of active aluminum in the nano aluminum powder for a long time and prevent the active aluminum from being oxidized; and 2, the Al/Ni composite particles are ignited by the ignition wire in the air atmosphere, the combustion speed is high, and the total combustion time of a 50mg sample placed in a conical shape is only about 450 ms.
Drawings
FIG. 1 is a 100nm TEM image of the Al/Ni composite particles.
FIG. 2 is a scanning electron micrograph of the Al/Ni composite particles at 500 nm.
FIG. 3 is a high-speed video recording of the combustion process of Al/Ni composite particles in an air atmosphere.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
Weighing 1.0g of nano aluminum powder, and weighing 40mL of absolute ethyl alcohol to prepare a suspension; weighing 0.5g of nickel chloride hexahydrate, weighing 50mL of absolute ethyl alcohol, and preparing into a transparent solution; adding the suspension into a transparent solution, and stirring to form a mixed turbid solution; weighing 0.12g of sodium hydroxide, weighing 15.0mL of absolute ethyl alcohol, and preparing a sodium hydroxide ethanol solution; and (3) dropwise adding the sodium hydroxide ethanol solution into the mixed turbid solution at 40 ℃, violently stirring for 10min, and carrying out suction filtration and vacuum drying at 50 ℃ to obtain a final product. The Al/Ni composite particles are found to have good dispersibility, the total combustion time of a 50mg sample placed as a cone is only 471ms, and the nano aluminum powder with the same specification is not ignited under the same condition.
Example 2
Weighing 0.5g of nano aluminum powder, weighing 20mL of absolute ethyl alcohol, and preparing into a suspension; weighing 0.25g of nickel sulfate, weighing 25mL of absolute ethyl alcohol, and preparing into a transparent solution; adding the suspension into a transparent solution, and stirring to form a mixed turbid solution; weighing 0.06g of sodium hydroxide, weighing 7.5mL of absolute ethyl alcohol, and preparing a sodium hydroxide ethanol solution; and (3) dropwise adding the sodium hydroxide ethanol solution into the mixed turbid solution at 25 ℃, violently stirring for 10min, and carrying out suction filtration and vacuum drying at 50 ℃ to obtain a final product. It was found that 50mg of the Al/Ni composite particles prepared at low temperature were placed in a cone with a total burning time of 753 ms.
Example 3
Weighing 1.0g of nano aluminum powder, and weighing 40mL of absolute ethyl alcohol to prepare a suspension; weighing 0.5g of nickel chloride hexahydrate, weighing 50mL of absolute ethyl alcohol, and preparing into a transparent solution; adding the suspension into a transparent solution, and stirring to form a mixed turbid solution; weighing 0.12g of sodium hydroxide, weighing 15.0mL of absolute ethyl alcohol, and preparing a sodium hydroxide ethanol solution; and (3) dropwise adding the sodium hydroxide ethanol solution into the mixed turbid solution at the temperature of 55 ℃, violently stirring for 10min, and carrying out suction filtration and vacuum drying at the temperature of 50 ℃ to obtain a final product. It was found that 50mg of the Al/Ni composite particles prepared under high temperature conditions were placed in a cone with a total combustion time of 697 ms.
Example 4
Weighing 0.5g of nano aluminum powder, weighing 20mL of absolute ethyl alcohol, and preparing into a suspension; weighing 0.25g of nickel sulfate, weighing 25mL of absolute ethyl alcohol, and preparing into a transparent solution; adding the suspension into a transparent solution, and stirring to form a mixed turbid solution; weighing 0.2g of sodium hydroxide, weighing 7.5mL of absolute ethyl alcohol, and preparing a sodium hydroxide ethanol solution; and (3) dropwise adding the sodium hydroxide ethanol solution into the mixed turbid solution at 40 ℃, violently stirring for 10min, and carrying out suction filtration and vacuum drying at 50 ℃ to obtain a final product. It was found that 50mg of the Al/Ni composite particles prepared with higher sodium hydroxide content, placed as cones, were not ignited under the same experimental conditions.
Example 5
Weighing 1.0g of nano aluminum powder, and weighing 40mL of absolute ethyl alcohol to prepare a suspension; weighing 0.8g of nickel chloride hexahydrate, weighing 50mL of absolute ethyl alcohol, and preparing into a transparent solution; adding the suspension into a transparent solution, and stirring to form a mixed turbid solution; weighing 0.12g of sodium hydroxide, weighing 15.0mL of absolute ethyl alcohol, and preparing a sodium hydroxide ethanol solution; and (3) dropwise adding the sodium hydroxide ethanol solution into the mixed turbid solution at 40 ℃, violently stirring for 10min, and carrying out suction filtration and vacuum drying at 50 ℃ to obtain a final product. The total combustion time of the Al/Ni composite particles prepared under the condition of higher nickel salt content when a 50mg sample is placed as a cone is 766 ms.
FIG. 1 is a transmission electron micrograph of the Al/Ni composite particles, and it can be seen that the composite particles have a typical core-shell structure.
FIG. 2 is a scanning electron micrograph of the Al/Ni composite particles, which shows that the composite particles have good micro-morphology.
Fig. 3 is a high-speed video recording of the combustion process of the Al/Ni composite particles in the air atmosphere, which is shot at a shooting rate of 2000 frames/second, and it can be seen that the composite particles have good combustion performance and a fast combustion rate.
Summarizing the above examples, it was found that the present invention can be achieved by controlling the conditions: the environment temperature of 35-45 ℃, the mass ratio of sodium hydroxide to aluminum powder of 1: 50-1: 5 and the mass ratio of nickel salt to aluminum powder of 1: 10-1: 2 are reasonable conditions for preparing the Al/Ni composite particles, and the combustion performance of the finally prepared composite particles is deteriorated by changing the environment temperature and the mass ratio of sodium hydroxide, aluminum powder and nickel salt, which is reflected in that the combustion time of a cone sample of 50mg is prolonged.

Claims (6)

1. An Al/Ni composite particle, characterized in that: the composite particle is composed of 3.6-14.8% of nickel by mass fraction, 68.7-96.0% of activated aluminum by mass fraction and 0.4-16.5% of alumina by mass fraction.
2. The Al/Ni composite particle according to claim 1, characterized in that: the composite particles are of a core-shell structure, the micro-nano aluminum powder is a core, and the nickel is coated on the surface of the aluminum powder.
3. A method for producing Al/Ni composite particles according to any one of claims 1 to 2, characterized in that: the method comprises the following steps: (1) weighing sodium hydroxide, and adding the sodium hydroxide into absolute ethyl alcohol to form a transparent solution; (2) weighing aluminum powder and nickel salt, adding the aluminum powder and nickel salt into absolute ethyl alcohol, and then carrying out ultrasonic dispersion for 30min to form uniform suspension; (3) transferring the transparent solution and the suspension prepared in the steps (1) and (2) into a constant-temperature water bath kettle, setting the water bath temperature to be 35-45 ℃, and enabling the temperatures of the transparent solution and the suspension to reach the set temperature; (4) dropwise adding the transparent solution prepared in the step (1) into the suspension prepared in the step (2), and violently stirring the suspension in the dropwise adding process, wherein the total reaction time is controlled to be 5-10 min; (5) and after the reaction is finished, carrying out suction filtration and vacuum drying, and collecting the composite particles.
4. The method for producing Al/Ni composite particles according to claim 3, characterized in that: the mass ratio of the sodium hydroxide to the aluminum powder is 1: 50-1: 5; the mass ratio of the nickel salt to the aluminum powder is 1: 10-1: 2.
5. The method for producing Al/Ni composite particles according to claim 3, characterized in that: the purity of the nickel salt is more than 99.9 percent.
6. The method for producing Al/Ni composite particles according to claim 3, characterized in that: the solvent used in the preparation process is absolute ethyl alcohol, and the purity is more than 99.9.
CN201910271798.6A 2019-04-04 2019-04-04 Al/Ni composite particles and preparation method thereof Active CN111774579B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114309593A (en) * 2021-09-24 2022-04-12 中北大学 Preparation method of multi-transition metal coated micron aluminum composite fuel
CN115477319A (en) * 2022-09-16 2022-12-16 无锡成旸科技股份有限公司 Anti-agglomeration composite powder and preparation method thereof

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JPS5891102A (en) * 1981-11-24 1983-05-31 Toda Kogyo Corp Production of magnetic particle powder of needle crystal alloy
CN101041180A (en) * 2007-04-28 2007-09-26 北京有色金属研究总院 Nanometer Al contained Ni and the preparing method
CN101181751A (en) * 2007-12-17 2008-05-21 中国铝业股份有限公司 Method for preparing nickel-coated alumina powder
CN101239390A (en) * 2007-02-09 2008-08-13 国家纳米技术与工程研究院 Method for preparing core-shell structure functional coating nano aluminium-nickel powder
CN103273061A (en) * 2013-06-08 2013-09-04 沈阳化工大学 Preparation method for electroplating dispersing agent nickel coated aluminum powder
CN103433485A (en) * 2013-08-16 2013-12-11 北京工业大学 Nickel package aluminum powder and preparing method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5891102A (en) * 1981-11-24 1983-05-31 Toda Kogyo Corp Production of magnetic particle powder of needle crystal alloy
CN101239390A (en) * 2007-02-09 2008-08-13 国家纳米技术与工程研究院 Method for preparing core-shell structure functional coating nano aluminium-nickel powder
CN101041180A (en) * 2007-04-28 2007-09-26 北京有色金属研究总院 Nanometer Al contained Ni and the preparing method
CN101181751A (en) * 2007-12-17 2008-05-21 中国铝业股份有限公司 Method for preparing nickel-coated alumina powder
CN103273061A (en) * 2013-06-08 2013-09-04 沈阳化工大学 Preparation method for electroplating dispersing agent nickel coated aluminum powder
CN103433485A (en) * 2013-08-16 2013-12-11 北京工业大学 Nickel package aluminum powder and preparing method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114309593A (en) * 2021-09-24 2022-04-12 中北大学 Preparation method of multi-transition metal coated micron aluminum composite fuel
CN114309593B (en) * 2021-09-24 2024-04-05 中北大学 Preparation method of multielement transition metal coated micron aluminum composite fuel
CN115477319A (en) * 2022-09-16 2022-12-16 无锡成旸科技股份有限公司 Anti-agglomeration composite powder and preparation method thereof

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