CN103318973B - 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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CN103318973B
CN103318973B CN201310259969.6A CN201310259969A CN103318973B CN 103318973 B CN103318973 B CN 103318973B CN 201310259969 A CN201310259969 A CN 201310259969A CN 103318973 B CN103318973 B CN 103318973B
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microballoon
coated
carbon
preparation
absorbing material
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CN103318973A (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

The coated Fe of a kind of carbon 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 absorption of electromagnetic wave field, but undressed Fe 3o 4usual specific inductivity is lower, and real part of permittivity is no more than 5, and imaginary part of dielectric constant is no more than 2.5, is difficult to realize impedance matching, and therefore absorption of electromagnetic wave performance is extremely restricted.For improving Fe 3o 4impedance matching property, need further to improve its specific inductivity.Carbonaceous material has higher specific inductivity, with Fe 3o 4prepare matrix material and not only greatly can improve Fe 3o 4specific inductivity, carbonaceous material is also common dielectric loss type radio-radar absorber, has good fade performance equally to microwave.Therefore by carbonaceous material is coated on Fe 3o 4the outer improvement that can realize absorption of electromagnetic wave performance.
Therefore, carbon material reasonable in design and Fe 3o 4the microtexture of composite microwave absorption agent, effectively can regulate the specific inductivity of matrix material, and introduces dielectric loss and magnetic loss simultaneously and decay to impinging microwave, has very big raising to absorbing property, and it is significant to expand its application.
Summary of the invention
The present invention will solve current 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 coated Fe 3o 4the preparation method of microballoon absorbing material.
The coated Fe of carbon of the present invention 3o 4the preparation method of microballoon absorbing material, carries out according to the following steps:
One, Fe is prepared 3o 4microballoon: by the FeCl of 1 ~ 5g 36H 2o dissolves in the organic solvent of 50 ~ 100mL, and stir to obtain solution A; The precipitation agent of 1 ~ 5g is dissolved in the organic solvent of 50 ~ 100mL, stir to obtain solution B, the solution A of gained is mixed with solution B, stirs, obtain mixing solutions, gained mixing solutions is loaded in tetrafluoroethylene autoclave, at 100 ~ 200 DEG C of reaction 12 ~ 24h, obtain product A, then first use distilled water wash products therefrom A, use absolute ethanol washing product A again, final drying obtains Fe 3o 4microballoon;
Two, the coated Fe of resol 3o 4the preparation of microballoon: the Fe that 0.5 ~ 2g step one is obtained 3o 4the solvent of 112.4mL put into by microballoon, carry out ultrasonic disperse, 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 room temperature, in reaction process, carry out mechanical stirring, obtain product B, then first use distilled water wash products therefrom B, then use absolute ethanol washing product B, final drying obtains the coated Fe of resol 3o 4microballoon;
Three, the coated Fe of carbon 3o 4the preparation of microballoon: by Fe coated for resol 3o 4microballoon is put into tube furnace and is carried out carbonization, with nitrogen or rare gas element for protection gas, is warming up to 400 ~ 800 DEG C, keeps 4h, obtain the Fe that carbon is coated with the speed of 1 ~ 5 DEG C/min 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, solves current carbon and Fe 3o 4class absorbing material is only the present situation of simple composite, realizes the specific inductivity being regulated matrix material by morphology design, improves impedance matching, strengthen the object of absorption of electromagnetic wave performance.Conventional Fe 3o 4the real part of permittivity scope of microballoon is less than 6, and imaginary part of dielectric constant is no more than 2.5; Carbon prepared by the present invention and Fe 3o 4the real part of permittivity of nucleocapsid structure absorbing material is greater than 18, and imaginary part of dielectric constant, is conducive to realizing impedance matching mainly about 0 at low frequency, strengthens absorbing property; The present invention prepares carbon and Fe 3o 4composite material of core-shell structure can be used for absorption of electromagnetic wave field.
Accompanying drawing explanation
Fig. 1 is the coated Fe of carbon prepared by embodiment 1 3o 4the electron scanning micrograph of microballoon; Fig. 2 is the coated Fe of carbon prepared by embodiment 1 3o 4fe in microballoon 3o 4dissolved the transmission electron microscope photo of rear carbon shell; Fig. 3 is the coated Fe of carbon prepared by embodiment 2 3o 4the electron scanning micrograph of microballoon; Fig. 4 is the coated Fe of carbon prepared by embodiment 2 3o 4fe in microballoon 3o 4dissolved the transmission electron microscope photo of rear carbon shell; Fig. 5 is the coated Fe of carbon prepared by embodiment 3 3o 4the electron scanning micrograph of microballoon; Fig. 6 is the coated Fe of carbon prepared by embodiment 3 3o 4fe in microballoon 3o 4dissolved the transmission electron microscope photo of rear carbon shell; Fig. 7 is the coated Fe of carbon prepared by embodiment 1,2 and 3 3o 4the XRD figure of microballoon; Fig. 8 is the coated Fe of carbon prepared by embodiment 4 3o 4the electron scanning micrograph of microballoon; Fig. 9 is the coated Fe of carbon prepared by embodiment 5 and embodiment 6 3o 4the real part of permittivity figure of microballoon; Figure 10 is the coated Fe of carbon prepared by embodiment 5 and embodiment 6 3o 4the imaginary part of dielectric constant figure of microballoon; Figure 11 is the coated Fe of carbon prepared by embodiment 7 and embodiment 8 3o 4the real part of permittivity figure of microballoon; Figure 12 is the coated Fe of carbon prepared by embodiment 7 and embodiment 8 3o 4the imaginary part of dielectric constant 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: the coated Fe of present embodiment carbon 3o 4the preparation method of microballoon absorbing material, carries out according to the following steps:
One, Fe is prepared 3o 4microballoon: by the FeCl of 1 ~ 5g 36H 2o dissolves in the organic solvent of 50 ~ 100mL, and stir to obtain solution A; The precipitation agent of 1 ~ 5g is dissolved in the organic solvent of 50 ~ 100mL, stir to obtain solution B, the solution A of gained is mixed with solution B, stirs, obtain mixing solutions, gained mixing solutions is loaded in tetrafluoroethylene autoclave, at 100 ~ 200 DEG C of reaction 12 ~ 24h, obtain product A, then first use distilled water wash products therefrom A, use absolute ethanol washing product A again, final drying obtains Fe 3o 4microballoon;
Two, the coated Fe of resol 3o 4the preparation of microballoon: the Fe that 0.5 ~ 2g step one is obtained 3o 4the solvent of 112.4mL put into by microballoon, carry out ultrasonic disperse, 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 room temperature, in reaction process, carry out mechanical stirring, obtain product B, then first use distilled water wash products therefrom B, then use absolute ethanol washing product B, final drying obtains the coated Fe of resol 3o 4microballoon;
Three, the coated Fe of carbon 3o 4the preparation of microballoon: by Fe coated for resol 3o 4microballoon is put into tube furnace and is carried out carbonization, with nitrogen or rare gas element for protection gas, is warming up to 400 ~ 800 DEG C, keeps 4h, obtain the Fe that carbon is coated with the speed of 1 ~ 5 DEG C/min 3o 4microballoon.
Embodiment two: present embodiment and embodiment one unlike: organic solvent described in step one be one or both in ethylene glycol, glycerol by arbitrarily than the mixture formed.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: precipitation agent described in step one be one or more in sodium acetate, anhydrous, crystallization sodium acetate, Trisodium Citrate by arbitrarily than the mixture formed.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: the ammoniacal liquor that solvent described in step 2 is 25% by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration forms.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: add the Resorcinol of 0.1 ~ 0.4g and the formaldehyde of 0.14 ~ 0.56mL in step 2 successively.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to four unlike: add the Resorcinol of 0.15 ~ 0.2g and the formaldehyde of 0.21 ~ 0.28mL in step 2 successively.Other is identical with one of embodiment one to four.
Embodiment seven: one of present embodiment and embodiment one to six unlike: be warming up to 600 ~ 700 DEG C with the speed of 2 ~ 4 DEG C/min in step 3.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to six unlike: be warming up to 650 DEG C with the speed of 3 DEG C/min in step 3.Other is identical with one of embodiment one to six.
Embodiment 1:
The coated Fe of the present embodiment carbon 3o 4the preparation method of microballoon absorbing material, carries out according to the following steps:
One, Fe is prepared 3o 4microballoon: by the FeCl of 2.7g 36H 2o dissolves in the ethylene glycol of 70mL, and stir to obtain solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir to obtain solution B, the solution A of gained is mixed with solution B, stirs, obtain mixing solutions, gained mixing solutions is loaded in tetrafluoroethylene autoclave, at 200 DEG C of reaction 24h, obtain product A, then first use distilled water wash products therefrom A to clarification of water, use absolute ethanol washing product A again, final drying obtains Fe 3o 4microballoon;
Two, the coated Fe of resol 3o 4the preparation of microballoon: the Fe that 1g step one is obtained 3o 4the solvent of 112.4mL put into by microballoon, carry out ultrasonic disperse, after being uniformly dispersed, add the Resorcinol of 0.6g and the formaldehyde of 0.84mL successively, under room temperature, react 24h, in reaction process, carry out mechanical stirring, obtain product B, then first use distilled water wash products therefrom B to clarification of water, then use absolute ethanol washing product B, final drying obtains the coated Fe of resol 3o 4microballoon;
Three, the coated Fe of carbon 3o 4the preparation of microballoon: by Fe coated for resol 3o 4microballoon is put into tube furnace and is carried out carbonization, with nitrogen or rare gas element for protection gas, is warming up to 650 DEG C, keeps 4h, obtain the Fe that carbon is coated with the speed of 3 DEG C/min 3o 4microballoon.The ammoniacal liquor that solvent described in step 2 is 25% by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration forms.
The Fe that the carbon prepared of the present embodiment is coated 3o 4the electron scanning micrograph of microballoon as shown in Figure 1, can find out that microballoon entirety presents spherical; By Fe coated for carbon 3o 4fe in microballoon 3o 4after dissolving with the concentrated hydrochloric acid of 12mol/L, the transmission electron microscope photo of carbon shell as shown in Figure 2, illustrates the Fe that carbon is coated 3o 4microballoon has obvious nucleocapsid structure.
Embodiment 2:
The coated Fe of the present embodiment carbon 3o 4the preparation method of microballoon absorbing material, carries out according to the following steps:
One, Fe is prepared 3o 4microballoon: by the FeCl of 2.7g 36H 2o dissolves in the ethylene glycol of 70mL, and stir to obtain solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir to obtain solution B, the solution A of gained is mixed with solution B, stirs, obtain mixing solutions, gained mixing solutions is loaded in tetrafluoroethylene autoclave, at 200 DEG C of reaction 24h, obtain product A, then first use distilled water wash products therefrom A to clarification of water, use absolute ethanol washing product A again, final drying obtains Fe 3o 4microballoon;
Two, the coated Fe of resol 3o 4the preparation of microballoon: the Fe that 1g step one is obtained 3o 4the solvent of 112.4mL put into by microballoon, carry out ultrasonic disperse, after being uniformly dispersed, add the Resorcinol of 0.4g and the formaldehyde of 0.56mL successively, under room temperature, react 24h, in reaction process, carry out mechanical stirring, obtain product B, then first use distilled water wash products therefrom B to clarification of water, then use absolute ethanol washing product B, final drying obtains the coated Fe of resol 3o 4microballoon;
Three, the coated Fe of carbon 3o 4the preparation of microballoon: by Fe coated for resol 3o 4microballoon is put into tube furnace and is carried out carbonization, with nitrogen or rare gas element for protection gas, is warming up to 650 DEG C, keeps 4h, obtain the Fe that carbon is coated with the speed of 3 DEG C/min 3o 4microballoon.The ammoniacal liquor that solvent described in step 2 is 25% by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration forms.
The Fe that the carbon prepared of the present embodiment is coated 3o 4the electron scanning micrograph of microballoon as shown in Figure 3, can find out that microballoon entirety presents spherical; By Fe coated for carbon 3o 4fe in microballoon 3o 4after dissolving with the concentrated hydrochloric acid of 12mol/L, the transmission electron microscope photo of carbon shell as shown in Figure 4, illustrates the Fe that carbon is coated 3o 4microballoon has obvious nucleocapsid structure.
Embodiment 3:
The coated Fe of the present embodiment carbon 3o 4the preparation method of microballoon absorbing material, carries out according to the following steps:
One, Fe is prepared 3o 4microballoon: by the FeCl of 2.7g 36H 2o dissolves in the ethylene glycol of 70mL, and stir to obtain solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir to obtain solution B, the solution A of gained is mixed with solution B, stirs, obtain mixing solutions, gained mixing solutions is loaded in tetrafluoroethylene autoclave, at 200 DEG C of reaction 24h, obtain product A, then first use distilled water wash products therefrom A to clarification of water, use absolute ethanol washing product A again, final drying obtains Fe 3o 4microballoon;
Two, the coated Fe of resol 3o 4the preparation of microballoon: the Fe that 1g step one is obtained 3o 4the solvent of 112.4mL put into by microballoon, carry out ultrasonic disperse, after being uniformly dispersed, add the Resorcinol of 0.2g and the formaldehyde of 0.28mL successively, under room temperature, react 24h, in reaction process, carry out mechanical stirring, obtain product B, then first use distilled water wash products therefrom B to clarification of water, then use absolute ethanol washing product B, final drying obtains the coated Fe of resol 3o 4microballoon;
Three, the coated Fe of carbon 3o 4the preparation of microballoon: by Fe coated for resol 3o 4microballoon is put into tube furnace and is carried out carbonization, with nitrogen or rare gas element for protection gas, is warming up to 650 DEG C, keeps 4h, obtain the Fe that carbon is coated with the speed of 3 DEG C/min 3o 4microballoon.The ammoniacal liquor that solvent described in step 2 is 25% by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration forms.
The Fe that the carbon prepared of the present embodiment is coated 3o 4the electron scanning micrograph of microballoon as shown in Figure 5, can find out that microballoon entirety presents spherical; By Fe coated for carbon 3o 4fe in microballoon 3o 4after dissolving with the concentrated hydrochloric acid of 12mol/L, the transmission electron microscope photo of carbon shell as shown in Figure 6, illustrates the Fe that carbon is coated 3o 4microballoon has obvious nucleocapsid structure.
The coated Fe of carbon prepared by embodiment 1,2 and 3 3o 4as shown in Figure 7, wherein curve a is the coated Fe of carbon prepared by embodiment 1 to the XRD figure of microballoon 3o 4the XRD curve of microballoon, curve b is the coated Fe of carbon prepared by embodiment 2 3o 4the XRD curve of microballoon, curve c is the coated Fe of carbon prepared by embodiment 3 3o 4the XRD curve of microballoon.Not assorted peak, illustrates that the material of preparation is very pure as seen from the figure.
Embodiment 4:
The coated Fe of the present embodiment carbon 3o 4the preparation method of microballoon absorbing material, carries out according to the following steps:
One, Fe is prepared 3o 4microballoon: by the FeCl of 2.7g 36H 2o dissolves in the ethylene glycol of 70mL, and stir to obtain solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir to obtain solution B, the solution A of gained is mixed with solution B, stirs, obtain mixing solutions, gained mixing solutions is loaded in tetrafluoroethylene autoclave, at 200 DEG C of reaction 24h, obtain product A, then first use distilled water wash products therefrom A to clarification of water, use absolute ethanol washing product A again, final drying obtains Fe 3o 4microballoon;
Two, the coated Fe of resol 3o 4the preparation of microballoon: the Fe that 1g step one is obtained 3o 4the solvent of 112.4mL put into by microballoon, carry out ultrasonic disperse, after being uniformly dispersed, add the Resorcinol of 0.1g and the formaldehyde of 0.14mL successively, under room temperature, react 24h, in reaction process, carry out mechanical stirring, obtain product B, then first use distilled water wash products therefrom B to clarification of water, then use absolute ethanol washing product B, final drying obtains the coated Fe of resol 3o 4microballoon;
Three, the coated Fe of carbon 3o 4the preparation of microballoon: by Fe coated for resol 3o 4microballoon is put into tube furnace and is carried out carbonization, with nitrogen or rare gas element for protection gas, is warming up to 650 DEG C, keeps 4h, obtain the Fe that carbon is coated with the speed of 3 DEG C/min 3o 4microballoon.The ammoniacal liquor that solvent described in step 2 is 25% by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration forms.
The Fe that the carbon prepared of the present embodiment is coated 3o 4the electron scanning micrograph of microballoon as shown in Figure 8, can find out that microballoon entirety presents spherical.
Embodiment 5:
The coated Fe of the present embodiment carbon 3o 4the preparation method of microballoon absorbing material, carries out according to the following steps:
One, Fe is prepared 3o 4microballoon: by the FeCl of 2.7g 36H 2o dissolves in the ethylene glycol of 70mL, and stir to obtain solution A; The sodium acetate, anhydrous of 5g is dissolved in the ethylene glycol of 30mL, stir to obtain solution B, the solution A of gained is mixed with solution B, stirs, obtain mixing solutions, gained mixing solutions is loaded in tetrafluoroethylene autoclave, at 200 DEG C of reaction 24h, obtain product A, then first use distilled water wash products therefrom A to clarification of water, use absolute ethanol washing product A again, final drying obtains Fe 3o 4microballoon;
Two, the coated Fe of resol 3o 4the preparation of microballoon: the Fe that 1g step one is obtained 3o 4the solvent of 112.4mL put into by microballoon, carry out ultrasonic disperse, after being uniformly dispersed, add the Resorcinol of 0.15g and the formaldehyde of 0.21mL successively, under room temperature, react 24h, in reaction process, carry out mechanical stirring, obtain product B, then first use distilled water wash products therefrom B to clarification of water, then use absolute ethanol washing product B, final drying obtains the coated Fe of resol 3o 4microballoon;
Three, the coated Fe of carbon 3o 4the preparation of microballoon: by Fe coated for resol 3o 4microballoon is put into tube furnace and is carried out carbonization, with nitrogen or rare gas element for protection gas, is warming up to 600 DEG C, keeps 4h, obtain the Fe that carbon is coated with the speed of 3 DEG C/min 3o 4microballoon.The ammoniacal liquor that solvent described in step 2 is 25% by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration forms.
Embodiment 6:
The present embodiment place different from embodiment 5 is to add the Resorcinol of 0.05g and the formaldehyde of 0.07mL in step 2 successively, and other are identical with embodiment 5.
Embodiment 7:
The present embodiment place different from embodiment 5 is to be warming up to 700 DEG C with the speed of 3 DEG C/min in step 3, and other are identical with embodiment 5.
Embodiment 8:
The present embodiment place different from embodiment 7 is to add the Resorcinol of 0.05g and the formaldehyde of 0.07mL in step 2 successively, and other are identical with embodiment 7.
The Fe that the carbon prepared of embodiment 5 and embodiment 6 is coated 3o 4the real part of permittivity of microballoon as shown in Figure 9, the Fe that the carbon prepared of embodiment 5 and embodiment 6 is coated 3o 4the imaginary part of dielectric constant of microballoon as shown in Figure 10, in Fig. 9 and Figure 10-zero-the coated Fe of carbon for preparing for embodiment 5 3o 4microballoon ,--for embodiment 6 prepare the coated Fe of carbon 3o 4microballoon;
The Fe that the carbon prepared of embodiment 7 and embodiment 8 is coated 3o 4the real part of permittivity of microballoon as shown in figure 11, the Fe that the carbon prepared of embodiment 7 and embodiment 8 is coated 3o 4the imaginary part of dielectric constant of microballoon as shown in figure 12, in Figure 11 and Figure 12-zero-the coated Fe of carbon for preparing for embodiment 7 3o 4microballoon ,--for embodiment 8 prepare the coated Fe of carbon 3o 4microballoon;
As can be seen from Fig. 9 to Figure 12, by Fe 3o 4carry out carbon coated after, its dielectric real part significantly improves, and can bring up to 18 (conventional Fe 3o 4the dielectric real part scope of microballoon is less than 6); Imaginary part of dielectric constant is also significantly improved (conventional Fe 3o 4the dielectric imaginary part of microballoon at low frequency mainly about 0), the therefore coated Fe of carbon 3o 4microballoon matrix material is conducive to realizing impedance matching, strengthens absorbing property.

Claims (5)

1. the coated Fe of carbon 3o 4the preparation method of microballoon absorbing material, is characterized in that the method is carried out according to the following steps:
One, Fe is prepared 3o 4microballoon: by the FeCl of 1 ~ 5g 36H 2o dissolves in the organic solvent of 50 ~ 100mL, and stir to obtain solution A; The precipitation agent of 1 ~ 5g is dissolved in the organic solvent of 50 ~ 100mL, stir to obtain solution B, the solution A of gained is mixed with solution B, stirs, obtain mixing solutions, gained mixing solutions is loaded in tetrafluoroethylene autoclave, at 100 ~ 200 DEG C of reaction 12 ~ 24h, obtain product A, then first use distilled water wash products therefrom A, use absolute ethanol washing product A again, final drying obtains Fe 3o 4microballoon;
Two, the coated Fe of resol 3o 4the preparation of microballoon: the Fe that 0.5 ~ 2g step one is obtained 3o 4the solvent of 112.4mL put into by microballoon, carry out ultrasonic disperse, 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 room temperature, in reaction process, carry out mechanical stirring, obtain product B, then first use distilled water wash products therefrom B, then use absolute ethanol washing product B, final drying obtains the coated Fe of resol 3o 4microballoon;
Three, the coated Fe of carbon 3o 4the preparation of microballoon: by Fe coated for resol 3o 4microballoon is put into tube furnace and is carried out carbonization, with nitrogen or rare gas element for protection gas, is warming up to 400 ~ 800 DEG C, keeps 4h, obtain the Fe that carbon is coated with the speed of 1 ~ 5 DEG C/min 3o 4microballoon; Wherein organic solvent described in step one is that one or both in ethylene glycol, glycerol are by arbitrarily than the mixture formed; Precipitation agent described in step one is that one or more in sodium acetate, anhydrous, crystallization sodium acetate, Trisodium Citrate are by arbitrarily than the mixture formed; The ammoniacal liquor that solvent described in step 2 is 25% by 80mL deionized water, 32mL dehydrated alcohol and 0.4mL mass concentration forms.
2. the coated Fe of a kind of carbon according to claim 1 3o 4the preparation method of microballoon absorbing material, is characterized in that adding the Resorcinol of 0.1 ~ 0.4g and the formaldehyde of 0.14 ~ 0.56mL in step 2 successively.
3. the coated Fe of a kind of carbon according to claim 1 3o 4the preparation method of microballoon absorbing material, is characterized in that adding the Resorcinol of 0.15 ~ 0.2g and the formaldehyde of 0.21 ~ 0.28mL in step 2 successively.
4. the coated Fe of a kind of carbon according to claim 1 3o 4the preparation method of microballoon absorbing material, is characterized in that being warming up to 600 ~ 700 DEG C with the speed of 2 ~ 4 DEG C/min in step 3.
5. the coated Fe of a kind of carbon according to claim 1 3o 4the preparation method of microballoon absorbing material, is characterized in that being warming up to 650 DEG C with the speed of 3 DEG C/min in 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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