CN108659790A - A kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene - Google Patents
A kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of the composite wave-suction material of magnetic-particle intercalation porous graphene, are as follows：S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action and expands layer；S2, the multilayer graphene oxide after expansion layer is dried；S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；S5, step S2 multilayer graphene oxides are added in the solution described in step S4；S6, the step S5 solution prepared is evaporated to drying；S7, the mixture for preparing step S6 carry out high-temperature process；S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, magnetic-particle intercalation porous graphene composite material is finally made in re-dry after cleaning.The present invention absorbing material high temperature resistance it is good, it is light-weight, inhale wave frequency bandwidth.
Description
Technical field
The invention belongs to graphenes to produce and process field, specifically, being related to a kind of magnetic-particle intercalation porous graphene
Composite wave-suction material preparation method.
Background technology
Graphene is as a kind of new carbon, because its higher dielectric constant and the easy dielectric relaxor of outer-shell electron are special
Property, it can be as dielectric loss substrate applications in suction wave field.
But existing graphene is during the manufacturing, its absorbing property of single dielectric loss Effect of Materials,
The performance for affecting graphene causes certain inconvenience to the use of people.
Invention content
1, it to solve the problems, such as
For the problem of existing grapheme material absorbing property difference, the purpose of the present invention is to provide a kind of magnetic-particles to insert
The preparation method of the composite wave-suction material of layer porous graphene, grapheme material is combined with magnetic-particle, to solve the above-mentioned back of the body
The problem of being proposed in scape technology.
2, technical solution
To achieve the above object, the present invention provides the following technical solutions：
A kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene, is as follows：
S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action
Expand layer, the microwave time is 1-100min；
S2, the multilayer graphene oxide after expansion layer is dried, drying temperature is 20-150 DEG C, drying time 10-
100min；
S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；
S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；
S5, step S2 multilayer graphene oxides are added in the solution described in step S4, ultrasonic disperse 10-500min；
S6, the step S5 solution prepared is evaporated to drying, obtains the mixture of graphene and metal salt；
S7, the mixture for preparing step S6 carry out high-temperature process, and temperature is 300-1500 DEG C, soaking time 10-
500min leads to N2 protections, ventilatory capacity 0.01-10m in the process3The graphite containing magnetic-particle intercalation is finally made in/hour
Alkene；
S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, at 40-150 DEG C after cleaning
Magnetic-particle intercalation porous graphene composite material is finally made in middle drying.
Preferably, the preparation method of the composite wave-suction material of above-mentioned magnetic-particle intercalation porous graphene, specific steps are such as
Under：
S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action
Expand layer, the microwave time is 10-90min；
S2, the multilayer graphene oxide after expansion layer is dried, drying temperature is 30-120 DEG C, drying time 20-
90min；
S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；
S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；
S5, step S2 multilayer graphene oxides are added in the solution described in step S4, ultrasonic disperse 50-400min；
S6, the step S5 solution prepared is evaporated to drying, obtains the mixture of graphene and metal salt；
S7, the mixture for preparing step S6 carry out high-temperature process, and temperature is 400-1200 DEG C, soaking time 20-
450min leads to N2 protections, ventilatory capacity 1-8m in the process3The graphene containing magnetic-particle intercalation is finally made in/hour；
S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, at 50-130 DEG C after cleaning
Magnetic-particle intercalation porous graphene composite material is finally made in middle drying.
Preferably, the preparation method of the composite wave-suction material of above-mentioned magnetic-particle intercalation porous graphene, specific steps are such as
Under：
S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action
Expand layer, the microwave time is 120min；
S2, the multilayer graphene oxide after expansion layer is dried, drying temperature is 60 DEG C, drying time 120min；
S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；
S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；
S5, step S2 multilayer graphene oxides are added in the solution described in step S4, ultrasonic disperse 120min；
S6, the step S5 solution prepared is evaporated to drying, obtains the mixture of graphene and metal salt；
S7, the mixture for preparing step S6 carry out high-temperature process, and temperature is 800 DEG C, soaking time 60min, process
In lead to N2Protection, ventilatory capacity 1m3The graphene containing magnetic-particle intercalation is finally made in/hour；
S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, is done in 60 DEG C after cleaning
It is dry, magnetic-particle intercalation porous graphene composite material is finally made.
Preferably, in the solution that prepared by the described step S1 mass fraction of multilayer graphene oxide be 0.01-10% it
Between.
Preferably, the mass fraction of ethyl alcohol is between 10-90% in the solution prepared in the step S3, tetrahydrofuran
For mass fraction between 10-90%, surplus is distilled water.
Preferably, the mass fraction of potassium hydroxide is between 0.01-30% in the solution that prepared by the step S4, levulinic
The mass fraction of ketone cobalt is between 0.01-30%, and the mass fraction of ferric acetyl acetonade is between 0.01-30%, nickel acetylacetonate
Mass fraction between 0.01-30%.
3, advantageous effect
Compared with prior art, the beneficial effects of the invention are as follows：
The preparation method of the present invention effectively combines graphene oxide with magnetic-particle, prepared layer and layer and
Surface all loads the porous graphene for the particle that is magnetic.The present invention absorbing material high temperature resistance it is good, it is light-weight, inhale wave frequency band
Width has good absorbing property within the scope of the radar wave of 2-40GHZ.
Specific implementation mode
Technical scheme of the present invention is described in more detail With reference to embodiment.
Embodiment 1
A kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene, is as follows：
S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action
Expand layer, the microwave time is 1min；
S2, the multilayer graphene oxide after expansion layer is dried, drying temperature is 60 DEG C, drying time 100min；
S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；
S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；
S5, step S2 multilayer graphene oxides are added in the solution described in step S4, ultrasonic disperse 60min；
S6, the step S5 solution prepared is evaporated to drying, obtains the mixture of graphene and metal salt；
S7, the mixture for preparing step S6 carry out high-temperature process, and temperature is 650 DEG C, soaking time 60min, process
In lead to N2 protection, ventilatory capacity 1m3The graphene containing alloy intercalation is finally made in/hour；
S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, is done in 60 DEG C after cleaning
It is dry, magnetic-particle intercalation porous graphene composite material is finally made.
The mass fraction of multilayer graphene oxide is between 0.01-10% in solution prepared by the step S1；
The mass fraction of ethyl alcohol is between 10-90% in the solution prepared in the step S3, the quality point of tetrahydrofuran
For number between 10-90%, surplus is distilled water；
The mass fraction of potassium hydroxide is between 0.01-30% in solution prepared by the step S4, acetylacetone cobalt
Mass fraction is between 0.01-30%, and the mass fraction of ferric acetyl acetonade is between 0.01-30%, the quality of nickel acetylacetonate
Score is between 0.01-30%.
Embodiment 2
A kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene, is as follows：
S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action
Expand layer, the microwave time is 50min；
S2, the multilayer graphene oxide after expansion layer is dried, drying temperature is 70 DEG C, drying time 80min；
S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；
S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；
S5, step S2 multilayer graphene oxides are added in the solution described in step S4, ultrasonic disperse 100min；
S6, the step S5 solution prepared is evaporated to drying, obtains the mixture of graphene and metal salt；
S7, the mixture for preparing step S6 carry out high-temperature process, and temperature is 800 DEG C, soaking time 30min, process
In lead to N2Protection, ventilatory capacity 2m3The graphene containing alloy intercalation is finally made in/hour；
S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, is done in 80 DEG C after cleaning
It is dry, magnetic-particle intercalation porous graphene composite material is finally made.
The mass fraction of multilayer graphene oxide is between 0.01-10% in solution prepared by the step S1；
The mass fraction of ethyl alcohol is between 10-90% in the solution prepared in the step S3, the quality point of tetrahydrofuran
For number between 10-90%, surplus is distilled water；
The mass fraction of potassium hydroxide is between 0.01-30% in solution prepared by the step S4, acetylacetone cobalt
Mass fraction is between 0.01-30%, and the mass fraction of ferric acetyl acetonade is between 0.01-30%, the quality of nickel acetylacetonate
Score is between 0.01-30%.
Embodiment 3
A kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene, is as follows：
S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action
Expand layer, the microwave time is 100min；
S2, the multilayer graphene oxide after expansion layer is dried, drying temperature is 80 DEG C, drying time 60min；
S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；
S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；
S5, step S2 multilayer graphene oxides are added in the solution described in step S4, ultrasonic disperse 150min；
S6, the step S5 solution prepared is evaporated to drying, obtains the mixture of graphene and metal salt；
S7, the mixture for preparing step S6 carry out high-temperature process, and temperature is 1000 DEG C, soaking time 30min, process
In lead to N2 protection, ventilatory capacity 5m3The graphene containing alloy intercalation is finally made in/hour；
S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, is done in 80 DEG C after cleaning
It is dry, magnetic-particle intercalation porous graphene composite material is finally made.
The mass fraction of multilayer graphene oxide is between 0.01-10% in solution prepared by the step S1；
The mass fraction of ethyl alcohol is between 10-90% in the solution prepared in the step S3, the quality point of tetrahydrofuran
For number between 10-90%, surplus is distilled water；
The mass fraction of potassium hydroxide is between 0.01-30% in solution prepared by the step S4, acetylacetone cobalt
Mass fraction is between 0.01-30%, and the mass fraction of ferric acetyl acetonade is between 0.01-30%, the quality of nickel acetylacetonate
Score is between 0.01-30%.
The better embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, one skilled in the relevant art within the scope of knowledge, can also be without departing from the purpose of the present invention
Various changes can be made.
Claims (6)
1. a kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene, which is characterized in that specific steps
It is as follows：
S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action and expands layer,
The microwave time is 1-100min；
S2, the multilayer graphene oxide after expansion layer is dried, drying temperature is 20-150 DEG C, drying time 10-
100min；
S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；
S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；
S5, step S2 multilayer graphene oxides are added in the solution described in step S4, ultrasonic disperse 10-500min；
S6, the step S5 solution prepared is evaporated to drying, obtains the mixture of graphene and metal salt；
S7, the mixture for preparing step S6 carry out high-temperature process, and temperature is 300-1500 DEG C, soaking time 10-500min,
Lead to N2 protections, ventilatory capacity 0.01-10m in the process3The graphene containing magnetic-particle intercalation is finally made in/hour；
S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, is done in 40-150 DEG C after cleaning
It is dry, magnetic-particle intercalation porous graphene composite material is finally made.
2. a kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene according to claim 1,
It is characterized in that, being as follows：
S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action and expands layer,
The microwave time is 10-90min；
S2, the multilayer graphene oxide after expansion layer is dried, drying temperature is 30-120 DEG C, drying time 20-
90min；
S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；
S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；
S5, step S2 multilayer graphene oxides are added in the solution described in step S4, ultrasonic disperse 50-400min；
S6, the step S5 solution prepared is evaporated to drying, obtains the mixture of graphene and metal salt；
S7, the mixture for preparing step S6 carry out high-temperature process, and temperature is 400-1200 DEG C, soaking time 20-450min,
Lead to N2 protections, ventilatory capacity 1-8m in the process3The graphene containing magnetic-particle intercalation is finally made in/hour；
S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, is done in 50-130 DEG C after cleaning
It is dry, magnetic-particle intercalation porous graphene composite material is finally made.
3. a kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene according to claim 1,
It is characterized in that, being as follows：
S1, multilayer graphene oxide is dissolved into distilled water, graphene layer expansion is then carried out under microwave field action and expands layer,
The microwave time is 50min；
S2, the multilayer graphene oxide after expansion layer is dried, drying temperature is 60 DEG C, drying time 120min；
S3, solvent of the configuration containing distilled water, ethyl alcohol and tetrahydrofuran；
S4, potassium hydroxide, acetylacetone cobalt, ferric acetyl acetonade, nickel acetylacetonate are added in solvent prepared by step S3；
S5, step S2 multilayer graphene oxides are added in the solution described in step S4, ultrasonic disperse 120min；
S6, the step S5 solution prepared is evaporated to drying, obtains the mixture of graphene and metal salt；
S7, the mixture for preparing step S6 carry out high-temperature process, and temperature is 800 DEG C, soaking time 60min, leads to N in the process2
Protection, ventilatory capacity 1m3The graphene containing magnetic-particle intercalation is finally made in/hour；
S8, the graphene obtained after the processing of step S7 high temperatures is cleaned with distilled water, it is dry in 60 DEG C after cleaning, most
Magnetic-particle intercalation porous graphene composite material is made afterwards.
4. a kind of composite wave-suction material of magnetic-particle intercalation porous graphene according to claim 1-3 any one
Preparation method, which is characterized in that the mass fraction of multilayer graphene oxide is 0.01- in solution prepared by the step S1
Between 10%.
5. a kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene according to claim 4,
It is characterized in that, the mass fraction of ethyl alcohol is between 10-90% in the solution prepared in the step S3, the quality of tetrahydrofuran
For score between 10-90%, surplus is distilled water.
6. a kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene according to claim 5,
It is characterized in that, the mass fraction of potassium hydroxide is between 0.01-30% in solution prepared by the step S4, acetylacetone cobalt
Mass fraction between 0.01-30%, the mass fraction of ferric acetyl acetonade is between 0.01-30%, the matter of nickel acetylacetonate
Score is measured between 0.01-30%.
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Cited By (1)
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| CN110295415A (en) * | 2019-06-28 | 2019-10-01 | 南通大学 | A kind of preparation method of intercalated graphite alkene/carbon fiber magnetism Wave suction composite material |
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| CN107325283A (en) * | 2017-07-21 | 2017-11-07 | 张娟 | A kind of soluble polyaniline doped graphene cladding nano nickel composite wave-suction material and preparation method thereof |
| CN107567272A (en) * | 2017-09-26 | 2018-01-09 | 南通大学 | A kind of absorbing carbon fiber wave material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106683813A (en) * | 2016-12-19 | 2017-05-17 | 北京工业大学 | Graphene-coated variable phase nano magnetic composite material and preparation method thereof |
| CN107325283A (en) * | 2017-07-21 | 2017-11-07 | 张娟 | A kind of soluble polyaniline doped graphene cladding nano nickel composite wave-suction material and preparation method thereof |
| CN107567272A (en) * | 2017-09-26 | 2018-01-09 | 南通大学 | A kind of absorbing carbon fiber wave material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110295415A (en) * | 2019-06-28 | 2019-10-01 | 南通大学 | A kind of preparation method of intercalated graphite alkene/carbon fiber magnetism Wave suction composite material |
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