CN103318973A - Preparation method of carbon-cladding Fe3O4 microsphere wave-absorbing material - Google Patents

Preparation method of carbon-cladding Fe3O4 microsphere wave-absorbing material Download PDF

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CN103318973A
CN103318973A CN2013102599696A CN201310259969A CN103318973A CN 103318973 A CN103318973 A CN 103318973A CN 2013102599696 A CN2013102599696 A CN 2013102599696A CN 201310259969 A CN201310259969 A CN 201310259969A CN 103318973 A CN103318973 A CN 103318973A
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microballoon
coats
preparation
carbon
absorbing material
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CN103318973B (en
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杜耘辰
刘文文
韩喜江
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention relates to a preparation method of a carbon-cladding Fe3O4 microsphere wave-absorbing material, and relates to a preparation method of a wave-absorbing material. The preparation method aims to solve the problem of poor electromagnet wave absorption because impedance match is difficult to realize due to lower dielectric constant of Fe3O4 at present. The method comprises the following steps of: 1, preparing a Fe3O4 microsphere; 2, preparing a phenolic resin-cladding Fe3O4 microsphere; 3, preparing a carbon-cladding Fe3O4 microsphere. The carbon and Fe3O4 core-shell structure wave-absorbing material prepared through the method disclosed by the invention achieves the real part of a dielectric constant more than 18 and the imaginary part of the dielectric constant mainly about 0 at low frequency, thereby being favorable to realizing the impedance match and enhancing the wave-absorbing property; the carbon and Fe3O4 core-shell structure composite material prepared through the method disclosed by the invention can be used for the field of electromagnet wave absorption.

Description

A kind of carbon coats Fe 3O 4The preparation method of microballoon absorbing material
Technical field
The present invention relates to a kind of preparation method of absorbing material.
Background technology
Fe 3O 4Be one of common Ferrite Material, and be widely used in the absorption of electromagnetic wave field, however undressed Fe 3O 4Usually specific inductivity is lower, and real part of permittivity is no more than 5, and the specific inductivity imaginary part is no more than 2.5, is difficult to realize impedance matching, so the absorption of electromagnetic wave performance is subjected to very big restriction.For improving Fe 3O 4Impedance matching property, need further to improve its specific inductivity.Carbonaceous material has higher dielectric constant, with Fe 3O 4The preparation matrix material not only can improve Fe greatly 3O 4Specific inductivity, carbonaceous material also are common dielectric loss type radio-radar absorbers, equally microwave are had good fade performance.Therefore by carbonaceous material is coated on Fe 3O 4The outer improvement that can realize the absorption of electromagnetic wave performance.
Therefore, carbon material and Fe reasonable in design 3O 4The microtexture of composite microwave absorption agent can effectively be regulated the specific inductivity of matrix material, and introduces dielectric loss simultaneously and magnetic loss decays to the incident microwave, and absorbing property is had very big raising, and it is significant to expand its application.
Summary of the invention
The present invention will solve present Fe 3O 4Specific inductivity is lower, is difficult to realize impedance matching, and causes the problem of electromagnetic wave absorbability difference, provides a kind of carbon to coat Fe 3O 4The preparation method of microballoon absorbing material.
Carbon of the present invention coats Fe 3O 4The preparation method of microballoon absorbing material, carry out according to the following steps:
One, preparation Fe 3O 4Microballoon: with the FeCl of 1～5g 36H 2O dissolves in the organic solvent of 50～100mL, stir solution A; The precipitation agent of 1～5g is dissolved in the organic solvent of 50～100mL, stir solution B, the solution A of gained is mixed with solution B, stir, get mixing solutions, the gained mixing solutions is packed in the tetrafluoroethylene autoclave, at 100～200 ℃ of reaction 12～24h, get product A, then earlier with distilled water wash products therefrom A, use the absolute ethanol washing product A again, final drying obtains Fe 3O 4Microballoon;
Two, resol coats Fe 3O 4The preparation of microballoon: with the Fe of 0.5～2g step 1 acquisition 3O 4Microballoon is put into the solvent of 112.4mL, carry out ultra-sonic dispersion, after being uniformly dispersed, add the Resorcinol of 0.05～0.6g and the formaldehyde of 0.07～0.84mL successively, react 12～48h under the room temperature, carry out mechanical stirring in the reaction process, get product B, earlier with distilled water wash products therefrom B, use the absolute ethanol washing product B more then, final drying obtains the Fe that resol coats 3O 4Microballoon;
Three, carbon coats Fe 3O 4The preparation of microballoon: with the Fe of resol coating 3O 4Microballoon is put into tube furnace and is carried out carbonization, serves as protection gas with nitrogen or rare gas element, is warming up to 400～800 ℃ with the speed of 1～5 ℃/min, keeps 4h, namely gets the Fe that carbon coats 3O 4Microballoon.
Advantage of the present invention is:
The present invention utilizes indirect synthesis technique to realize carbon and Fe 3O 4The preparation of composite wave-suction material has solved current carbon and Fe 3O 4The class absorbing material only is the present situation of simple composite, realizes regulating by pattern and structure design the specific inductivity of matrix material, improves impedance matching, strengthens the purpose of absorption of electromagnetic wave performance.Conventional Fe 3O 4The real part of permittivity scope of microballoon is less than 6, and the specific inductivity imaginary part is no more than 2.5; Carbon and the Fe of the present invention's preparation 3O 4The real part of permittivity of nucleocapsid structure absorbing material is greater than 18, and the specific inductivity imaginary part mainly about 0, is conducive to realize impedance matching at low frequency, strengthens absorbing property; The present invention prepares carbon and Fe 3O 4Composite material of core-shell structure can be used for the absorption of electromagnetic wave field.
Description of drawings
Fig. 1 is the Fe that the carbon of embodiment 1 preparation coats 3O 4The electron scanning micrograph of microballoon; Fig. 2 is the Fe that the carbon of embodiment 1 preparation coats 3O 4Fe in the microballoon 3O 4The transmission electron microscope photo of dissolved back carbon shell; Fig. 3 is the Fe that the carbon of embodiment 2 preparations coats 3O 4The electron scanning micrograph of microballoon; Fig. 4 is the Fe that the carbon of embodiment 2 preparations coats 3O 4Fe in the microballoon 3O 4The transmission electron microscope photo of dissolved back carbon shell; Fig. 5 is the Fe that the carbon of embodiment 3 preparations coats 3O 4The electron scanning micrograph of microballoon; Fig. 6 is the Fe that the carbon of embodiment 3 preparations coats 3O 4Fe in the microballoon 3O 4The transmission electron microscope photo of dissolved back carbon shell; Fig. 7 is the Fe that the carbon of embodiment 1,2 and 3 preparations coats 3O 4The XRD figure of microballoon; Fig. 8 is the Fe that the carbon of embodiment 4 preparations coats 3O 4The electron scanning micrograph of microballoon; Fig. 9 is the Fe that the carbon of embodiment 5 and embodiment 6 preparations coats 3O 4The real part of permittivity figure of microballoon; Figure 10 is the Fe that the carbon of embodiment 5 and embodiment 6 preparations coats 3O 4The specific inductivity imaginary part figure of microballoon; Figure 11 is the Fe that the carbon of embodiment 7 and embodiment 8 preparations coats 3O 4The real part of permittivity figure of microballoon; Figure 12 is the Fe that the carbon of embodiment 7 and embodiment 8 preparations coats 3O 4The specific inductivity imaginary part figure of microballoon.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: present embodiment carbon coats Fe 3O 4The preparation method of microballoon absorbing material, carry out according to the following steps:
One, preparation Fe 3O 4Microballoon: with the FeCl of 1～5g 36H 2O dissolves in the organic solvent of 50～100mL, stir solution A; The precipitation agent of 1～5g is dissolved in the organic solvent of 50～100mL, stir solution B, the solution A of gained is mixed with solution B, stir, get mixing solutions, the gained mixing solutions is packed in the tetrafluoroethylene autoclave, at 100～200 ℃ of reaction 12～24h, get product A, then earlier with distilled water wash products therefrom A, use the absolute ethanol washing product A again, final drying obtains Fe 3O 4Microballoon;
Two, resol coats Fe 3O 4The preparation of microballoon: with the Fe of 0.5～2g step 1 acquisition 3O 4Microballoon is put into the solvent of 112.4mL, carry out ultra-sonic dispersion, after being uniformly dispersed, add the Resorcinol of 0.05～0.6g and the formaldehyde of 0.07～0.84mL successively, react 12～48h under the room temperature, carry out mechanical stirring in the reaction process, get product B, earlier with distilled water wash products therefrom B, use the absolute ethanol washing product B more then, final drying obtains the Fe that resol coats 3O 4Microballoon;
Three, carbon coats Fe 3O 4The preparation of microballoon: with the Fe of resol coating 3O 4Microballoon is put into tube furnace and is carried out carbonization, serves as protection gas with nitrogen or rare gas element, is warming up to 400～800 ℃ with the speed of 1～5 ℃/min, keeps 4h, namely gets the Fe that carbon coats 3O 4Microballoon.
Embodiment two: what present embodiment and embodiment one were different is: organic solvent described in the step 1 be in ethylene glycol, the glycerol one or both by any than mixtures of forming.Other is identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is: precipitation agent described in the step 1 is one or more mixtures formed by any ratio in sodium acetate, anhydrous, crystallization sodium acetate, the Trisodium Citrate.Other is identical with embodiment one or two.
Embodiment four: what present embodiment was different with one of embodiment one to three is: solvent described in the step 2 is that 25% ammoniacal liquor is formed by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration.Other is identical with one of embodiment one to three.
Embodiment five: what present embodiment was different with one of embodiment one to four is: add the Resorcinol of 0.1～0.4g and the formaldehyde of 0.14～0.56mL in the step 2 successively.Other is identical with one of embodiment one to four.
Embodiment six: what present embodiment was different with one of embodiment one to four is: add the Resorcinol of 0.15～0.2g and the formaldehyde of 0.21～0.28mL in the step 2 successively.Other is identical with one of embodiment one to four.
Embodiment seven: what present embodiment was different with one of embodiment one to six is: the speed with 2～4 ℃/min in the step 3 is warming up to 600～700 ℃.Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different with one of embodiment one to six is: the speed with 3 ℃/min in the step 3 is warming up to 650 ℃.Other is identical with one of embodiment one to six.
Embodiment 1:
Present embodiment carbon coats Fe 3O 4The preparation method of microballoon absorbing material, carry out according to the following steps:
One, preparation Fe 3O 4Microballoon: with the FeCl of 2.7g 36H 2O dissolves in the ethylene glycol of 70mL, stir solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir solution B, the solution A of gained is mixed with solution B, stir, get mixing solutions, the gained mixing solutions is packed in the tetrafluoroethylene autoclave, at 200 ℃ of reaction 24h, get product A, use distilled water wash products therefrom A to clarification of water then earlier, use the absolute ethanol washing product A again, final drying obtains Fe 3O 4Microballoon;
Two, resol coats Fe 3O 4The preparation of microballoon: with the Fe of 1g step 1 acquisition 3O 4Microballoon is put into the solvent of 112.4mL, carry out ultra-sonic dispersion, after being uniformly dispersed, add the Resorcinol of 0.6g and the formaldehyde of 0.84mL successively, react 24h under the room temperature, carry out mechanical stirring in the reaction process, get product B, use distilled water wash products therefrom B to clarification of water then earlier, use the absolute ethanol washing product B again, final drying obtains the Fe that resol coats 3O 4Microballoon;
Three, carbon coats Fe 3O 4The preparation of microballoon: with the Fe of resol coating 3O 4Microballoon is put into tube furnace and is carried out carbonization, serves as protection gas with nitrogen or rare gas element, is warming up to 650 ℃ with the speed of 3 ℃/min, keeps 4h, namely gets the Fe that carbon coats 3O 4Microballoon.The described solvent of step 2 is that 25% ammoniacal liquor is formed by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration.
The Fe that the carbon of present embodiment preparation coats 3O 4The electron scanning micrograph of microballoon as shown in Figure 1, microballoon integral body presents sphere as can be seen; Fe with the carbon coating 3O 4Fe in the microballoon 3O 4With the transmission electron microscope photo of the concentrated hydrochloric acid of 12mol/L dissolving back carbon shell as shown in Figure 2, the Fe of carbon coating be described 3O 4Microballoon has tangible nucleocapsid structure.
Embodiment 2:
Present embodiment carbon coats Fe 3O 4The preparation method of microballoon absorbing material, carry out according to the following steps:
One, preparation Fe 3O 4Microballoon: with the FeCl of 2.7g 36H 2O dissolves in the ethylene glycol of 70mL, stir solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir solution B, the solution A of gained is mixed with solution B, stir, get mixing solutions, the gained mixing solutions is packed in the tetrafluoroethylene autoclave, at 200 ℃ of reaction 24h, get product A, use distilled water wash products therefrom A to clarification of water then earlier, use the absolute ethanol washing product A again, final drying obtains Fe 3O 4Microballoon;
Two, resol coats Fe 3O 4The preparation of microballoon: with the Fe of 1g step 1 acquisition 3O 4Microballoon is put into the solvent of 112.4mL, carry out ultra-sonic dispersion, after being uniformly dispersed, add the Resorcinol of 0.4g and the formaldehyde of 0.56mL successively, react 24h under the room temperature, carry out mechanical stirring in the reaction process, get product B, use distilled water wash products therefrom B to clarification of water then earlier, use the absolute ethanol washing product B again, final drying obtains the Fe that resol coats 3O 4Microballoon;
Three, carbon coats Fe 3O 4The preparation of microballoon: with the Fe of resol coating 3O 4Microballoon is put into tube furnace and is carried out carbonization, serves as protection gas with nitrogen or rare gas element, is warming up to 650 ℃ with the speed of 3 ℃/min, keeps 4h, namely gets the Fe that carbon coats 3O 4Microballoon.The described solvent of step 2 is that 25% ammoniacal liquor is formed by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration.
The Fe that the carbon of present embodiment preparation coats 3O 4The electron scanning micrograph of microballoon as shown in Figure 3, microballoon integral body presents sphere as can be seen; Fe with the carbon coating 3O 4Fe in the microballoon 3O 4With the transmission electron microscope photo of the concentrated hydrochloric acid of 12mol/L dissolving back carbon shell as shown in Figure 4, the Fe of carbon coating be described 3O 4Microballoon has tangible nucleocapsid structure.
Embodiment 3:
Present embodiment carbon coats Fe 3O 4The preparation method of microballoon absorbing material, carry out according to the following steps:
One, preparation Fe 3O 4Microballoon: with the FeCl of 2.7g 36H 2O dissolves in the ethylene glycol of 70mL, stir solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir solution B, the solution A of gained is mixed with solution B, stir, get mixing solutions, the gained mixing solutions is packed in the tetrafluoroethylene autoclave, at 200 ℃ of reaction 24h, get product A, use distilled water wash products therefrom A to clarification of water then earlier, use the absolute ethanol washing product A again, final drying obtains Fe 3O 4Microballoon;
Two, resol coats Fe 3O 4The preparation of microballoon: with the Fe of 1g step 1 acquisition 3O 4Microballoon is put into the solvent of 112.4mL, carry out ultra-sonic dispersion, after being uniformly dispersed, add the Resorcinol of 0.2g and the formaldehyde of 0.28mL successively, react 24h under the room temperature, carry out mechanical stirring in the reaction process, get product B, use distilled water wash products therefrom B to clarification of water then earlier, use the absolute ethanol washing product B again, final drying obtains the Fe that resol coats 3O 4Microballoon;
Three, carbon coats Fe 3O 4The preparation of microballoon: with the Fe of resol coating 3O 4Microballoon is put into tube furnace and is carried out carbonization, serves as protection gas with nitrogen or rare gas element, is warming up to 650 ℃ with the speed of 3 ℃/min, keeps 4h, namely gets the Fe that carbon coats 3O 4Microballoon.The described solvent of step 2 is that 25% ammoniacal liquor is formed by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration.
The Fe that the carbon of present embodiment preparation coats 3O 4The electron scanning micrograph of microballoon as shown in Figure 5, microballoon integral body presents sphere as can be seen; Fe with the carbon coating 3O 4Fe in the microballoon 3O 4With the transmission electron microscope photo of the concentrated hydrochloric acid of 12mol/L dissolving back carbon shell as shown in Figure 6, the Fe of carbon coating be described 3O 4Microballoon has tangible nucleocapsid structure.
The Fe that the carbon of embodiment 1,2 and 3 preparations coats 3O 4The XRD figure of microballoon as shown in Figure 7, wherein curve a is the Fe that the carbon of embodiment 1 preparation coats 3O 4The XRD curve of microballoon, curve b are the Fe that the carbon of embodiment 2 preparations coats 3O 4The XRD curve of microballoon, curve c are the Fe that the carbon of embodiment 3 preparations coats 3O 4The XRD curve of microballoon.Not assorted peak exists as seen from the figure, illustrates that the material of preparation is very pure.
Embodiment 4:
Present embodiment carbon coats Fe 3O 4The preparation method of microballoon absorbing material, carry out according to the following steps:
One, preparation Fe 3O 4Microballoon: with the FeCl of 2.7g 36H 2O dissolves in the ethylene glycol of 70mL, stir solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir solution B, the solution A of gained is mixed with solution B, stir, get mixing solutions, the gained mixing solutions is packed in the tetrafluoroethylene autoclave, at 200 ℃ of reaction 24h, get product A, use distilled water wash products therefrom A to clarification of water then earlier, use the absolute ethanol washing product A again, final drying obtains Fe 3O 4Microballoon;
Two, resol coats Fe 3O 4The preparation of microballoon: with the Fe of 1g step 1 acquisition 3O 4Microballoon is put into the solvent of 112.4mL, carry out ultra-sonic dispersion, after being uniformly dispersed, add the Resorcinol of 0.1g and the formaldehyde of 0.14mL successively, react 24h under the room temperature, carry out mechanical stirring in the reaction process, get product B, use distilled water wash products therefrom B to clarification of water then earlier, use the absolute ethanol washing product B again, final drying obtains the Fe that resol coats 3O 4Microballoon;
Three, carbon coats Fe 3O 4The preparation of microballoon: with the Fe of resol coating 3O 4Microballoon is put into tube furnace and is carried out carbonization, serves as protection gas with nitrogen or rare gas element, is warming up to 650 ℃ with the speed of 3 ℃/min, keeps 4h, namely gets the Fe that carbon coats 3O 4Microballoon.The described solvent of step 2 is that 25% ammoniacal liquor is formed by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration.
The Fe that the carbon of present embodiment preparation coats 3O 4The electron scanning micrograph of microballoon as shown in Figure 8, microballoon integral body presents sphere as can be seen.
Embodiment 5:
Present embodiment carbon coats Fe 3O 4The preparation method of microballoon absorbing material, carry out according to the following steps:
One, preparation Fe 3O 4Microballoon: with the FeCl of 2.7g 36H 2O dissolves in the ethylene glycol of 70mL, stir solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir solution B, the solution A of gained is mixed with solution B, stir, get mixing solutions, the gained mixing solutions is packed in the tetrafluoroethylene autoclave, at 200 ℃ of reaction 24h, get product A, use distilled water wash products therefrom A to clarification of water then earlier, use the absolute ethanol washing product A again, final drying obtains Fe 3O 4Microballoon;
Two, resol coats Fe 3O 4The preparation of microballoon: with the Fe of 1g step 1 acquisition 3O 4Microballoon is put into the solvent of 112.4mL, carry out ultra-sonic dispersion, after being uniformly dispersed, add the Resorcinol of 0.15g and the formaldehyde of 0.21mL successively, react 24h under the room temperature, carry out mechanical stirring in the reaction process, get product B, use distilled water wash products therefrom B to clarification of water then earlier, use the absolute ethanol washing product B again, final drying obtains the Fe that resol coats 3O 4Microballoon;
Three, carbon coats Fe 3O 4The preparation of microballoon: with the Fe of resol coating 3O 4Microballoon is put into tube furnace and is carried out carbonization, serves as protection gas with nitrogen or rare gas element, is warming up to 600 ℃ with the speed of 3 ℃/min, keeps 4h, namely gets the Fe that carbon coats 3O 4Microballoon.The described solvent of step 2 is that 25% ammoniacal liquor is formed by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration.
Embodiment 6:
Present embodiment and embodiment 5 different places are to add successively in the step 2 Resorcinol of 0.05g and the formaldehyde of 0.07mL, and other are identical with embodiment 5.
Embodiment 7:
Present embodiment and embodiment 5 different places are that the speed with 3 ℃/min is warming up to 700 ℃ in the step 3, and other are identical with embodiment 5.
Embodiment 8:
Present embodiment and embodiment 7 different places are to add successively in the step 2 Resorcinol of 0.05g and the formaldehyde of 0.07mL, and other are identical with embodiment 7.
The Fe that the carbon of embodiment 5 and embodiment 6 preparations coats 3O 4The real part of permittivity of microballoon as shown in Figure 9, the Fe that the carbon of embodiment 5 and embodiment 6 preparations coats 3O 4The specific inductivity imaginary part of microballoon as shown in figure 10, among Fig. 9 and Figure 10-zero-be that the carbon of embodiment 5 preparations coats Fe 3O 4Microballoon ,--be the carbon coating Fe of embodiment 6 preparations 3O 4Microballoon;
The Fe that the carbon of embodiment 7 and embodiment 8 preparations coats 3O 4The real part of permittivity of microballoon as shown in figure 11, the Fe that the carbon of embodiment 7 and embodiment 8 preparations coats 3O 4The specific inductivity imaginary part of microballoon as shown in figure 12, among Figure 11 and Figure 12-zero-be that the carbon of embodiment 7 preparations coats Fe 3O 4Microballoon ,--be the carbon coating Fe of embodiment 8 preparations 3O 4Microballoon;
By Fig. 9 to Figure 12 as can be seen, with Fe 3O 4After carrying out the carbon coating, its dielectric real part obviously improves, and can bring up to 18 (conventional Fe 3O 4The dielectric real part scope of microballoon is less than 6); Specific inductivity imaginary part (the conventional Fe that also is significantly improved 3O 4The dielectric imaginary part of microballoon at low frequency mainly about 0), so carbon coats Fe 3O 4The microballoon matrix material is conducive to realize impedance matching, strengthens absorbing property.

Claims (8)

1. a carbon coats Fe 3O 4The preparation method of microballoon absorbing material is characterized in that this method carries out according to the following steps:
One, preparation Fe 3O 4Microballoon: with the FeCl of 1～5g 36H 2O dissolves in the organic solvent of 50～100mL, stir solution A; The precipitation agent of 1～5g is dissolved in the organic solvent of 50～100mL, stir solution B, the solution A of gained is mixed with solution B, stir, get mixing solutions, the gained mixing solutions is packed in the tetrafluoroethylene autoclave, at 100～200 ℃ of reaction 12～24h, get product A, then earlier with distilled water wash products therefrom A, use the absolute ethanol washing product A again, final drying obtains Fe 3O 4Microballoon;
Two, resol coats Fe 3O 4The preparation of microballoon: with the Fe of 0.5～2g step 1 acquisition 3O 4Microballoon is put into the solvent of 112.4mL, carry out ultra-sonic dispersion, after being uniformly dispersed, add the Resorcinol of 0.05～0.6g and the formaldehyde of 0.07～0.84mL successively, react 12～48h under the room temperature, carry out mechanical stirring in the reaction process, get product B, earlier with distilled water wash products therefrom B, use the absolute ethanol washing product B more then, final drying obtains the Fe that resol coats 3O 4Microballoon;
Three, carbon coats Fe 3O 4The preparation of microballoon: with the Fe of resol coating 3O 4Microballoon is put into tube furnace and is carried out carbonization, serves as protection gas with nitrogen or rare gas element, is warming up to 400～800 ℃ with the speed of 1～5 ℃/min, keeps 4h, namely gets the Fe that carbon coats 3O 4Microballoon.
2. a kind of carbon according to claim 1 coats Fe 3O 4The preparation method of microballoon absorbing material is characterized in that organic solvent described in the step 1 is one or both mixtures formed by any ratio in ethylene glycol, the glycerol.
3. a kind of carbon according to claim 1 coats Fe 3O 4The preparation method of microballoon absorbing material is characterized in that precipitation agent described in the step 1 is one or more mixtures formed by any ratio in sodium acetate, anhydrous, crystallization sodium acetate, the Trisodium Citrate.
4. a kind of carbon according to claim 1 coats Fe 3O 4The preparation method of microballoon absorbing material is characterized in that solvent described in the step 2 is that 25% ammoniacal liquor is formed by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration.
5. a kind of carbon according to claim 1 coats Fe 3O 4The preparation method of microballoon absorbing material is characterized in that adding successively in the step 2 Resorcinol of 0.1～0.4g and the formaldehyde of 0.14～0.56mL.
6. a kind of carbon according to claim 1 coats Fe 3O 4The preparation method of microballoon absorbing material is characterized in that adding successively in the step 2 Resorcinol of 0.15～0.2g and the formaldehyde of 0.21～0.28mL.
7. a kind of carbon according to claim 1 coats Fe 3O 4The preparation method of microballoon absorbing material is characterized in that the speed with 2～4 ℃/min is warming up to 600～700 ℃ in the step 3.
8. a kind of carbon according to claim 1 coats Fe 3O 4The preparation method of microballoon absorbing material is characterized in that the speed with 3 ℃/min is warming up to 650 ℃ in the step 3.
CN201310259969.6A 2013-06-26 2013-06-26 Preparation method of carbon-cladding Fe3O4 microsphere wave-absorbing material Expired - Fee Related CN103318973B (en)

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