CN105896099A - Method for preparing porous carbon ball composite absorbing material loaded with magnetic metal element - Google Patents
Method for preparing porous carbon ball composite absorbing material loaded with magnetic metal element Download PDFInfo
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- CN105896099A CN105896099A CN201610261067.XA CN201610261067A CN105896099A CN 105896099 A CN105896099 A CN 105896099A CN 201610261067 A CN201610261067 A CN 201610261067A CN 105896099 A CN105896099 A CN 105896099A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
Abstract
The invention relates to a method for preparing a porous carbon ball composite absorbing material loaded with a magnetic metal element. The method includes the steps of 1] preparing a precursor solution containing magnetic metal ion salt; 2] placing porous carbon balls into the precursor solution for stirring and dipping; 3] filtering, then washing and drying the porous carbon balls; 4] calcining the dried porous carbon balls in an inert atmosphere; and 5] cooling to room temperature in the inert atmosphere and then obtaining a porous carbon ball composite absorbing material loaded with a magnetic metal element. The invention makes use of the high specific surface area and the strong adsorption of the porous carbon balls, introduces the precursor solution containing magnetic metal ion salt including cobalt salt, nickel salt and the like into channels of the carbon balls by capillary action, combines with hydrophilic oxygen-containing functional groups, and obtains the porous carbon ball composite absorbing material loaded with the magnetic metal element like cobalt or nickel through drying and sintering in the inert atmosphere. The whole preparation process is simple in technique, convenient to operate, and less demanding on production equipment.
Description
Technical field
The present invention relates to the preparation method of a kind of composite wave-suction material, be specifically related to a kind of carried magnetic metal list
The preparation method of the porous carbon ball composite radar wave absorbing material of matter.
Background technology
Along with aggravation and the quickening of IT application process of modern war electronic countermeasure, the development of absorbing material just court
The direction high performance is developed.From the point of view of the current result of study to absorbing material, complex technique becomes real
The prefered method of existing New Type Radar absorbing material " thin, light, wide, strong " design concept, be specifically related to by
Material based on electrical loss is (such as silicon carbide fibre, CNT, white carbon black, conduction high polymer and carbon fiber
Deng) be combined with the traditional magnetic material (such as magnetic metal micropowder and ferrite etc.) based on magnetic loss.
On the one hand, above-mentioned electrical loss absorbing material density is little, can realize lightweight as carrier；On the other hand, by electricity
Loss and magnetic loss material are combined and can reach multiband, wide band assimilation effect.Relevant suction ripple material
The research comparative maturity of material, also has much for electrical loss, the patent of magnetic loss complex technique and document,
Such as:
Wang etc., with coiled carbon fibers as carrier, use ALD (ald) technology by magnetic components
Fe3O4/ Ni granule " tiles " on CNT tube wall, can adjust material by the thickness of regulation and control magnetic component
The electromagnetic consumable of material entirety reaches optimum matching point, and the microwave that prepared composite granule has excellence is anti-
Penetrate loss.(see document: ACS Nano.2012 6 11009-11017.)
Wen etc. are many after ferric nitrate, cobalt salt and nickel salt aqueous solution being respectively enterd process by chemical impregnation
In wall carbon nano tube, in H after drying process2The lower 900 DEG C of reduction of atmosphere respectively obtain carried metal Fe,
The composite wave-suction material of Co and Ni, this material has the microwave absorption effect of excellence in S-band (2-4GHz)
Really, maximum reflection loss successively up to-39 ,-37 ,-37dB.(see document: J.Phys.Chem.C 2011,
115,14025–14030)
Ni etc. are by Co and the γ-Al of ball milling commercialization under inert atmosphere2O3Directly prepare Co/Al2O3Nanometer
Complex, the ratio regulating the two can control the electromagnetic parameter of complex, and then realize damaging microwave reflection
The optimization of consumption, obtains the microwave absorption effect of optimum.(see document: Journal of Alloys and
Compounds.2013,558,62-67.)
Bright reds etc. use the method for chemical plating that CNT carries out plated surface Ni, and the thickness of coating is about
8-15nm, result shows, along with the increase of matching thickness, the absworption peak of chemical nickel plating CNT is not sent out
Raw mobile, when matching thickness d=0.2mm, the minimum reflection loss of sample reaches-10.5dB.(see document:
Functional material [J] 2007,38 (7): 1213-1216.)
Yuan etc. by after the commercial acidified process of SiC, hydrophilic treated, photosensitive process and activation processing,
In surface of SiC, one layer of nickel salt " is covered " again by chemical deposition process, the most available through subsequent heat treatment
The SiC powder body that Ni modifies, this composite granule is expected to be used for high temperature absorbing material field.(list of references: Powder
Technology.2013,237,309-313.)
In the existing method for preparing composite wave-suction material, big multipair production equipment requirements is the highest, work
Skill process is complicated, and the problem that generally existence yields poorly, cost is high, it is only applicable to laboratory research, difficult
To realize large-scale production and application.
Summary of the invention
In order to solve existing composite wave-suction material preparation method and yield poorly, cost is high, the technology of complex process
Problem, the present invention provides a kind of technique to be simple and convenient to operate, less demanding load magnetic to the equipment of production
The preparation method of the porous carbon ball composite wave-suction material of property metal simple-substance.
The technical solution of the present invention is: the porous carbon ball of the carried magnetic metal simple-substance provided is compound to be inhaled
The preparation method of wave material comprises the following steps:
1] preparation precursor solution containing magnetic metal ion salt；
2] porous carbon ball is placed in described precursor solution stirring dipping；
3] after being leached by porous carbon ball, washing is dried；
4] dried porous carbon ball is calcined under an inert atmosphere；
5] the porous carbon ball composite wave-absorbing of carried magnetic metal simple-substance is obtained after being cooled to room temperature under an inert atmosphere
Material.
Above-mentioned steps 1] in precursor solution be to be dissolved in cobalt salt or nickel salt in deionized water to be prepared into
Arriving, the quality of cobalt salt or nickel salt is 2-6g:10-30ml with the ratio of the volume of deionized water.
Above-mentioned steps 2] comprise the following steps:
2.1] being placed in nitric acid by porous carbon ball, the quality of porous carbon ball is 1g with the ratio of the volume of nitric acid:
15-30ml；
2.2] stirring dipping 10-12h under water bath condition；
2.3] dried for washing porous carbon ball is placed in described precursor solution stirring dipping 12-24 hour,
The quality of porous carbon ball is 1-3g:9-20ml with the ratio of the volume of precursor solution.
Above-mentioned steps 2.1] in the mass fraction of nitric acid be 40-60%.
Above-mentioned steps 2.2] in the temperature of water-bath be 40-60 DEG C.
Above-mentioned steps 2.3] in washing be dried condition be repeatedly to clean to neutrality with deionized water, then put
100-110 DEG C of dry 12-24h in baking oven.
Above-mentioned steps 3] in washing be dried condition be repeatedly to clean with deionized water, be subsequently placed in baking oven
Middle 60-80 DEG C of dry 12-20h.
Above-mentioned steps 4] in calcination condition be 700-1000 DEG C of calcining at constant temperature 2-3 hour.
Above-mentioned inert atmosphere is nitrogen atmosphere or argon gas atmosphere.
Above-mentioned steps 2] in the diameter range of porous carbon ball be 0.5-2mm, BET specific surface area is
800-1300m2/ g, total hole volume is 0.4-0.9cm3/g。
The beneficial effects of the present invention is:
(1) present invention utilizes the high-specific surface area of porous carbon ball and strong adsorption by the magnetic such as cobalt salt, nickel salt
Metal cation salt precursor solution is incorporated into internal and oxygen-containing with the hydrophilic official in duct of carbon ball by capillarity
Group can combine, eventually pass sintering processes under dry, inert atmosphere and obtain the magnetic metal list such as Supported Co or nickel
The porous carbon ball composite of matter.Whole preparation process technique is simple, easy to operate, the equipment of production
Ask the highest.
(2) magnetic metal simple substance cobalt or nickel purity obtained by the present invention are high, and particle diameter is little and particle size distribution is equal
Even.It is carried on porous carbon ball and plays catalytic action, promote the degree of graphitization of carbon ball and improve material entirety
Dielectric properties.
(3) primary raw material used in the present invention is porous carbon ball, nitric acid, cobalt salt and nickel salt, is cost
General chemistry reagent cheap, that be readily available, is suitable for large-scale production and application.
Accompanying drawing explanation
Fig. 1 is the metal cobalt loaded porous carbon ball composite wave-suction material that the embodiment of the present invention one prepares
X ray diffracting spectrum；
Fig. 2 is the porous carbon ball composite wave-suction material of the carried metal nickel that the embodiment of the present invention two prepares
X ray diffracting spectrum；
Fig. 3 is the porous carbon ball composite wave-suction material of the carried metal nickel that the embodiment of the present invention two prepares
Raman collection of illustrative plates；
Fig. 4 is that the metal cobalt loaded porous carbon ball composite wave-suction material that the embodiment of the present invention three prepares exists
The electromagnetic wave absorption curve of Different matching layer thickness；
Fig. 5 is that the porous carbon ball composite wave-suction material of the carried metal nickel that the embodiment of the present invention four prepares exists
The electromagnetic wave absorption curve of Different matching layer thickness；
Detailed description of the invention
The present invention relates to the preparation side of the porous carbon ball composite radar wave absorbing material of a kind of carried magnetic metal simple-substance
Method.Primary raw material is porous carbon ball, nitric acid, cobalt salt and nickel salt.The method utilizes the Gao Bibiao of porous carbon ball
Cobalt salt, nickel salt precursor solution are incorporated in the duct of carbon ball by area and strong adsorption by capillarity
Portion is also combined with hydrophilic oxygen-containing functional group, eventually passes sintering processes under dry, inert atmosphere and obtains load
The porous carbon ball composite of magnetic metal simple substance.The magnetic components such as metal cobalt loaded or nickel on porous carbon ball
And the graphited amorphous carbon of part, magnetic components is 1:10～2:5 with the mass ratio of carrier carbon ball, porous
The BET specific surface area of carbon ball composite is 300-600m2/ g, particle diameter is distributed in 0.1-2.1mm.Metallic cobalt,
Nickel is elemental stage, is present in porous carbon ball inside and surface, plays catalytic action, promotes the graphitization of carbon ball
Degree also improves the dielectric properties that material is overall, the maximum microwave reflection loss of this composite wave-suction material up to
-25dB.The inventive method is simultaneously available for preparing other magnetic composite, and such absorbing material has height
Effect, the advantage of light weight, have broad application prospects in electromagnetic shielding and lightweight radar absorbing.Below
Property to the absorbing material that preparation method and use the method for the present invention prepare in conjunction with specific embodiments
Can be further explained.
Embodiment one
(1) particle diameter is distributed in the porous carbon ball of 0.5-2mm, and to be placed in the nitric acid that mass fraction is 40-60% molten
In liquid, the quality of carbon ball and nitric acid volume ratio are 1g:15-30ml, then stir under 40-60 DEG C of water bath condition
Mix dipping 10-12h, repeatedly clean to neutrality with deionized water, then in baking oven 100-110 DEG C be dried
12-24h；
(2) take cobalt salt to be dissolved in deionized water, prepare precursor solution, the quality of cobalt salt and deionized water
Volume ratio is 2-6g:10-30ml；
(3) porous carbon ball is immersed in above-mentioned precursor solution respectively, stirring dipping 12-24 hour, carbon ball
Quality is 1-3g:9-20ml with the volume ratio of precursor solution；
(4) porous carbon ball is leached from solution, use 10-40ml deionized water wash, filter；
(5) (4) gained porous carbon ball is put into 60-80 DEG C of dry 12-20h in baking oven；
(6) dried porous carbon ball is placed in tube furnace, forges in 1000 DEG C of constant temperature under an argon atmosphere
Burning 2-3 hour, continue to be cooled to room temperature under this atmosphere, the porous carbon ball obtaining carried metal simple substance cobalt is multiple
Close absorbing material.
Seeing Fig. 1, the thing phase main constituent obtaining product under this embodiment is simple substance Co, particle diameter about 15nm,
Being uniformly distributed in inside carbon ball, the specific surface area of complex is 305m2/g。
Embodiment two
(1) particle diameter is distributed in the porous carbon ball of 0.5-2mm, and to be placed in the nitric acid that mass fraction is 40-60% molten
In liquid, the quality of carbon ball and nitric acid volume ratio are 1g:15-30ml, then stir under 40-60 DEG C of water bath condition
Mix dipping 10-12h, repeatedly clean to neutrality with deionized water, then in baking oven 100-110 DEG C be dried
12-24h；
(2) take nickel salt to be dissolved in respectively in deionized water, prepare precursor solution, the quality of nickel salt and deionization
The volume ratio of water is 2-6g:10-30ml；
(3) porous carbon ball is immersed in above-mentioned precursor solution respectively, stirring dipping 12-24 hour, carbon ball
Quality is 1-3g:9-20ml with the volume ratio of precursor solution；
(4) porous carbon ball is leached from solution, use 10-40ml deionized water wash, filter；
(5) (4) gained porous carbon ball is put into 60-80 DEG C of dry 12-20h in baking oven；
(6) dried porous carbon ball is placed in tube furnace, in a nitrogen atmosphere in 900 DEG C of calcining at constant temperature
2-3 hour, continuing to be cooled to room temperature under this atmosphere, the porous carbon ball obtaining carried metal elemental nickel is combined
Absorbing material.
See Fig. 2 and Fig. 3, obtain the thing of product under this embodiment based on simple substance Ni, particle diameter about 25nm,
Being uniformly distributed in inside carbon ball, the degree of graphitization of complex is about 1.05.
Embodiment three
(1) particle diameter is distributed in the porous carbon ball of 0.5-2mm, and to be placed in the nitric acid that mass fraction is 40-60% molten
In liquid, the quality of carbon ball and nitric acid volume ratio are 1g:15-30ml, then stir under 40-60 DEG C of water bath condition
Mix dipping 10-12h, repeatedly clean to neutrality with deionized water, then in baking oven 100-110 DEG C be dried
12-24h；
(2) take cobalt salt to be dissolved in deionized water, prepare precursor solution, the quality of cobalt salt and deionized water
Volume ratio is 2-6g:10-30ml；
(3) porous carbon ball is immersed in above-mentioned precursor solution respectively, stirring dipping 12-24 hour, carbon ball
Quality is 1-3g:9-20ml with the volume ratio of precursor solution；
(4) porous carbon ball is leached from solution, use 10-40ml deionized water wash, filter；
(5) (4) gained porous carbon ball is put into 60-80 DEG C of dry 12-20h in baking oven；
(6) dried porous carbon ball is placed in tube furnace, under an argon atmosphere in 800 DEG C of calcining at constant temperature
2-3 hour, continuing to be cooled to room temperature under this atmosphere, the porous carbon ball obtaining carried metal simple substance cobalt is combined
Absorbing material.
See Fig. 4, obtain the thing phase composition of product under this embodiment based on simple substance Co, the ratio table of complex
Area is 400m2/ g, when simulating microwave absorbing coating thickness more than 4.5mm, on reflection loss curve
(2-18GHz) biabsorption peak occur, minimum reflection loss value when coating layer thickness is 5.5mm is-24.6dB.
Embodiment four
(1) particle diameter is distributed in the porous carbon ball of 0.5-2mm, and to be placed in the nitric acid that mass fraction is 40-60% molten
In liquid, the quality of carbon ball and nitric acid volume ratio are 1g:15-30ml, then stir under 40-60 DEG C of water bath condition
Mix dipping 10-12h, repeatedly clean to neutrality with deionized water, then in baking oven 100-110 DEG C be dried
12-24h；
(2) take nickel salt to be dissolved in respectively in deionized water, prepare precursor solution, the quality of nickel salt and deionization
The volume ratio of water is 2-6g:10-30ml；
(3) porous carbon ball is immersed in above-mentioned precursor solution respectively, stirring dipping 12-24 hour, carbon ball
Quality is 1-3g:9-20ml with the volume ratio of precursor solution；
(4) porous carbon ball is leached from solution, use 10-40ml deionized water wash, filter；
(5) (4) gained porous carbon ball is put into 60-80 DEG C of dry 12-20h in baking oven；
(6) dried porous carbon ball is placed in tube furnace, in a nitrogen atmosphere in 800 DEG C of calcining at constant temperature
2-3 hour, continuing to be cooled to room temperature under this atmosphere, the porous carbon ball obtaining carried metal elemental nickel is combined
Absorbing material.
Seeing Fig. 5, the thing phase composition obtaining product under this embodiment is divided into simple substance Ni, the specific surface of complex
Amass as 420m2/ g, when simulating microwave absorbing coating thickness more than 4.5mm, on reflection loss curve
(2-18GHz) biabsorption peak occur, minimum reflection loss value when coating layer thickness is 5.5mm is-21.5dB.
Claims (10)
1. a preparation method for the porous carbon ball composite wave-suction material of carried magnetic metal simple-substance, its feature exists
In: comprise the following steps:
1] preparation precursor solution containing magnetic metal ion salt；
2] porous carbon ball is placed in described precursor solution stirring dipping；
3] after being leached by porous carbon ball, washing is dried；
4] dried porous carbon ball is calcined under an inert atmosphere；
5] the porous carbon ball composite wave-absorbing of carried magnetic metal simple-substance is obtained after being cooled to room temperature under an inert atmosphere
Material.
The system of the porous carbon ball composite wave-suction material of carried magnetic metal simple-substance the most according to claim 1
Preparation Method, it is characterised in that: described step 1] in precursor solution be that cobalt salt or nickel salt are dissolved in
Preparing in deionized water, the quality of cobalt salt or nickel salt is 2-6g with the ratio of the volume of deionized water:
10-30ml。
The system of the porous carbon ball composite wave-suction material of carried magnetic metal simple-substance the most according to claim 2
Preparation Method, it is characterised in that: described step 2] comprise the following steps:
2.1] being placed in nitric acid by porous carbon ball, the quality of porous carbon ball is 1g with the ratio of the volume of nitric acid:
15-30ml；
2.2] stirring dipping 10-12h under water bath condition；
2.3] dried for washing porous carbon ball is placed in described precursor solution stirring dipping 12-24 hour,
The quality of porous carbon ball is 1-3g:9-20ml with the ratio of the volume of precursor solution.
The system of the porous carbon ball composite wave-suction material of carried magnetic metal simple-substance the most according to claim 3
Preparation Method, it is characterised in that: described step 2.1] in the mass fraction of nitric acid be 40-60%.
The system of the porous carbon ball composite wave-suction material of carried magnetic metal simple-substance the most according to claim 3
Preparation Method, it is characterised in that: described step 2.2] in the temperature of water-bath be 40-60 DEG C.
The system of the porous carbon ball composite wave-suction material of carried magnetic metal simple-substance the most according to claim 3
Preparation Method, it is characterised in that: described step 2.3] in washing be dried condition be the most clear with deionized water
It is washed till neutrality, is subsequently placed in 100-110 DEG C of dry 12-24h in baking oven.
7. according to the porous carbon ball composite wave-absorbing of described carried magnetic metal simple-substance arbitrary in claim 1-6
The preparation method of material, it is characterised in that: described step 3] in washing be dried condition be to use deionization
Water cleans repeatedly, is subsequently placed in 60-80 DEG C of dry 12-20h in baking oven.
The system of the porous carbon ball composite wave-suction material of carried magnetic metal simple-substance the most according to claim 7
Preparation Method, it is characterised in that: described step 4] in calcination condition be 700-1000 DEG C of calcining at constant temperature 2-3
Hour.
The system of the porous carbon ball composite wave-suction material of carried magnetic metal simple-substance the most according to claim 8
Preparation Method, it is characterised in that: described inert atmosphere is nitrogen atmosphere or argon gas atmosphere.
The porous carbon ball composite wave-suction material of carried magnetic metal simple-substance the most according to claim 9
Preparation method, it is characterised in that: described step 2] in the diameter range of porous carbon ball be 0.5-2mm,
BET specific surface area is 800-1300m2/ g, total hole volume is 0.4-0.9cm3/g。
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| CN108024493A (en) * | 2017-12-07 | 2018-05-11 | 广东工业大学 | A kind of mesoporous carbon of seedpod of the lotus structure and nanometer cobalt compound and its preparation method and application |
| CN108617154A (en) * | 2018-04-16 | 2018-10-02 | 晋中学院 | A kind of porous carbon load nano nickel absorbing material and preparation method thereof |
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Application publication date: 20160824 |