CN115636443A - Preparation method of magnetic nanoparticle coated microcapsule-shaped carbon-based composite material - Google Patents
Preparation method of magnetic nanoparticle coated microcapsule-shaped carbon-based composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 72
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 42
- 239000002122 magnetic nanoparticle Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 26
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- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 13
- 238000000576 coating method Methods 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 238000001354 calcination Methods 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 15
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 15
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- -1 ferric oxide compound Chemical class 0.000 claims description 11
- 238000006116 polymerization reaction Methods 0.000 claims description 10
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- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
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- FYFFGSSZFBZTAH-UHFFFAOYSA-N methylaminomethanetriol Chemical compound CNC(O)(O)O FYFFGSSZFBZTAH-UHFFFAOYSA-N 0.000 claims description 2
- 239000011258 core-shell material Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000011247 coating layer Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 47
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- PUAQLLVFLMYYJJ-UHFFFAOYSA-N 2-aminopropiophenone Chemical compound CC(N)C(=O)C1=CC=CC=C1 PUAQLLVFLMYYJJ-UHFFFAOYSA-N 0.000 description 1
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a magnetic nanoparticle coated microcapsule-shaped carbon-based composite material, belonging to the technical field of composite materials; the microcapsule-shaped carbon-based composite wave-absorbing material is of a core-shell coating structure and consists of a microcapsule-shaped ferric oxide template core prepared by mixing ferric iron metal salt, a sodium hydroxide aqueous solution and a sodium sulfate aqueous solution and a polydopamine carbon-based coating layer. According to the method, the microcapsule-shaped ferric oxide core is synthesized, polydopamine is coated on the surface of the microcapsule-shaped ferric oxide core by taking the microcapsule-shaped ferric oxide core as a template, and the mixture coated with the polydopamine is calcined at high temperature to prepare the magnetic nanoparticle-coated microcapsule-shaped carbon-based composite wave-absorbing material.
Description
Technical Field
The invention relates to a preparation method of a magnetic nanoparticle-coated carbon-based composite wave-absorbing material, in particular to a preparation method of a magnetic nanoparticle-coated microcapsule-shaped carbon-based composite material, belonging to the technical field of composite materials.
Background
With the development of modern science and technology, a large number of electronic products and communication equipment are widely applied, and serious electromagnetic radiation pollution is generated while convenience is provided for human life. Electromagnetic radiation pollution can not only affect the normal operation of various electronic equipment, but also cause long-term harm to human health, so that the application of the high-performance microwave absorbing material is one of the main means for solving the electromagnetic radiation pollution. Particularly in the military field, the development of radar stealth materials capable of efficiently absorbing electromagnetic waves is one of effective ways for improving the survivability of weapon systems.
The magnetic nano material has the advantages of wide raw material shaking, low cost, low preparation technology threshold and the like, so that different magnetic wave-absorbing materials with special compositions, structures and appearances are developed successively. However, the magnetic wave-absorbing material also has the defects of easy agglomeration, large density, poor high-temperature characteristic and the like, and in order to solve the problem, the carbon material and novel magnetic particles are prepared into a composite wave-absorbing material in the existing research, and the carbon material has the advantages of low cost, light weight and good conductivity. For example, patent document No. CN109014245B, wherein a monodisperse glycerol metal complex precursor is prepared by solvothermal method, and then in-situ polymerization of a nitrogen-containing organic monomer is utilized to coat the surface of the precursor to form a shell, and finally, the shell is calcined under inert gas, and the shell is carbonized to form nitrogen-doped carbon, and simultaneously the inner core is thermally decomposed to form magnetic nanoparticles, so as to prepare the coated magnetic nanoparticle composite material, but the preparation process is complex, and the carbon layer is not uniform; for example, the published DOI 10.1016/j carbon.2019.10.030 teaches a method for preparing a coated magnetic nanoparticle composite material, specifically, fe is prepared by a solvothermal method 2 O 3 The shape of the ring is such that,reuse of H 2 Reducing the mixed gas at high temperature to obtain Fe 3 O 4 Circularly carrying out the processes of polyvinylpyrrolidone (PVP) carbon source surface adsorption and high-temperature carbonization to prepare the core-shell structure Fe 3 O 4 the-C composite wave-absorbing material has complex preparation process and uses inflammable and explosive high-risk gas H 2 The wave-absorbing performance of the composite material can not meet the requirement.
Therefore, there is a need to design a carbon-based composite wave-absorbing material coated with magnetic nanoparticles, which has good wave-absorbing performance.
Disclosure of Invention
The purpose of the invention is: the composite wave-absorbing material is prepared by coating poly dopamine on the surface of a microcapsule-shaped ferric oxide template core, has good impedance matching performance and attenuation performance, and can fully absorb and attenuate electromagnetic waves to achieve the loss effect.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a magnetic nanoparticle coated microcapsule-shaped carbon-based composite material comprises the following steps:
s1, preparing a microcapsule template core: stirring ferric iron metal salt with the concentration of 2mol/L for 30min at the temperature of 75 ℃, dropwise adding sodium hydroxide aqueous solution with the concentration of 3-6 mol/L, continuously stirring for 30min, then adding sodium sulfate aqueous solution with the concentration of 0.5-1mol/L, uniformly mixing, injecting the mixed solution into a reaction kettle, putting the reaction kettle into an oven for reaction, washing the obtained product with deionized water to be neutral, performing suction filtration, and performing freeze drying to obtain a microcapsule-shaped ferric oxide template core;
s2, carrying out chemical polymerization coating on the surface of the template core: uniformly dispersing the microcapsule-shaped ferric oxide template core prepared in the step S1 into a trihydroxymethyl aminomethane aqueous solution with the pH =8.5, adding dopamine hydrochloride, stirring and reacting for 6h at room temperature, wherein the mass ratio of the ferric oxide template core to the dopamine hydrochloride is 1; washing the obtained product with deionized water and ethanol for 3 times respectively, performing suction filtration and drying to obtain a polydopamine-coated ferric oxide compound;
s3, calcining to prepare the composite wave-absorbing material: and (3) placing the polydopamine-coated ferric oxide composite powder prepared in the step (S2) into a tubular furnace, and calcining at a high temperature of 500-900 ℃ for 2-6 h in an inert atmosphere to obtain the magnetic nanoparticle-coated microcapsule-shaped carbon-based composite material.
In the step S1, the molar concentration of the sodium hydroxide aqueous solution is preferably 5.4mol/L, and the molar concentration of the sodium sulfate aqueous solution is preferably 0.6mol/L.
In the step S1, the ferric iron metal salt is ferric trichloride with crystal water.
In the step S1, the temperature of an oven is 100 to 120 ℃, the reaction time is 48 to 96h, the optimal temperature is 110 ℃, and the optimal reaction time is 72h.
In the step S2, preferably, the mass ratio of the ferric oxide template core to the dopamine hydrochloride is 1.
In the step S2, preferably, the calcination temperature is 750 ℃ and the calcination time is 4 hours.
The invention has the beneficial effects that:
1) The preparation method comprises the steps of obtaining a microcapsule-shaped ferric oxide template core by utilizing a simple hydrothermal process, obtaining a polydopamine-coated ferric oxide compound by a chemical polymerization coating process with dopamine hydrochloride, reducing the ferric oxide into ferroferric oxide magnetic particles by high temperature, and pyrolyzing the polydopamine into a carbon coating layer at the same time to obtain a product, namely the microcapsule-shaped carbon-based composite material coated with the magnetic nanoparticles.
2) The X-ray diffraction, raman spectrum and scanning electron microscope show that the coated magnetic nanoparticle microcapsule-like carbon-based composite material is successfully prepared by the method, electromagnetic parameter test of a network vector analyzer and wave absorption data obtained by Matlab simulation performance in the later period all prove that the coated magnetic nanoparticle microcapsule-like carbon-based composite material has good wave absorption performance, and the prepared coated magnetic nanoparticle microcapsule-like carbon-based composite material has good impedance matching performance and attenuation performance, can fully absorb and attenuate electromagnetic waves and achieves the loss effect.
Drawings
FIG. 1 shows Fe prepared in example 1 of the present invention 3 O 4 Scanning electron micrographs of @ C composite;
FIG. 2 shows Fe prepared in example 1 of the present invention 3 O 4 The Raman spectrogram of the @ C composite material;
FIG. 3 shows Fe prepared in example 1 of the present invention 3 O 4 X-ray diffraction patterns of @ C composites;
FIG. 4 shows Fe prepared in example 1 of the present invention 3 O 4 The reflection loss plot for the @ C composite;
FIG. 5 is Fe prepared in example 1~6 of the present invention 3 O 4 The reflection loss curve plot of d =1.8mm at the same thickness for the @ C composite.
Detailed Description
The invention is further explained below with reference to the figures and the embodiments.
Example 1: a preparation method of a magnetic nanoparticle coated microcapsule-shaped carbon-based composite material comprises the following steps:
s1, preparing a microcapsule template core: stirring 250mL of ferric trichloride with crystal water at the concentration of 2mol/L for 30min at the temperature of 75 ℃, dropwise adding 250mL of sodium hydroxide aqueous solution at the concentration of 5.4mol/L, continuously stirring for 30min, then adding 25mL of sodium sulfate aqueous solution at the concentration of 0.6mol/L, uniformly mixing, injecting the mixed solution into a reaction kettle, putting the reaction kettle into an oven for reaction, wherein the oven temperature is 110 ℃, the reaction time is 72h, washing the obtained product with deionized water to be neutral, performing suction filtration, and freeze drying to obtain the microcapsule-shaped ferric oxide (Fe) 2 O 3 -1) a template core;
s2, performing chemical polymerization coating on the surface of the template core: 0.1g of Fe 2 O 3 -1, uniformly dispersing template cores in a tris (hydroxymethyl) aminomethane aqueous solution with the pH =8.5, adding 0.05g dopamine hydrochloride, stirring and reacting for 6h at room temperature; washing the obtained product with deionized water and ethanol for 3 times respectively, filtering, and drying to obtain polydopamine-coated ferric oxide compound(Fe 2 O 3 @PDA-1);
S3, calcining to prepare the composite wave-absorbing material: mixing Fe 2 O 3 Putting the @ PDA-1 compound powder into a tubular furnace, and calcining at 750 ℃ for 4h in an inert atmosphere at high temperature to obtain the magnetic nanoparticle coated microcapsule-like carbon-based composite material (Fe) 3 O 4 @C-1)。
FIG. 1 is Fe 3 O 4 Scanning electron micrograph of @ C-1 composite, from which it can be seen that Fe 3 O 4 The @ C-1 composite material has an obvious microcapsule-like appearance and has a unique hollow core-shell structure;
FIG. 2 is Fe 3 O 4 The Raman spectrogram of the @ C-1 composite wave-absorbing material shows that Fe 3 O 4 The @ C-1 composite wave-absorbing material has obvious D peak and G peak, which indicates that the final product contains graphite carbon;
FIG. 3 is Fe 3 O 4 X-ray diffraction spectrum, peak position and Fe of @ C-1 composite wave-absorbing material 3 O 4 Is consistent with the standard PDF card of 26.0 0 No carbon diffraction peak appears nearby, indicating that amorphous carbon exists;
FIG. 4 is Fe 3 O 4 The reflection loss curve chart of the @ C-1 composite wave-absorbing material can show that Fe 3 O 4 The @ C composite has a minimum reflection loss value at a thickness of 4.0 mm.
Example 2: a preparation method of a magnetic nanoparticle coated microcapsule-shaped carbon-based composite material comprises the following steps:
s1, preparing a microcapsule template core: stirring 250mL of ferric trichloride with 2mol/L concentration and crystal water at 75 ℃ for 30min, dropwise adding 250mL of sodium hydroxide aqueous solution with 3mol/L concentration, continuously stirring for 30min, then adding 25mL of sodium sulfate aqueous solution with 0.5mol/L concentration, uniformly mixing, injecting the mixed solution into a reaction kettle, placing the reaction kettle into an oven for reaction at 100 ℃, wherein the reaction time is 96h, washing the obtained product with deionized water to be neutral, performing suction filtration, and freeze-drying to obtain microcapsule-shaped ferric oxide (Fe) 2 O 3 -2) template core;
S2, performing chemical polymerization coating on the surface of the template core: 0.1g of Fe 2 O 3 -1, uniformly dispersing template cores in a tris (hydroxymethyl) aminomethane aqueous solution with the pH =8.5, adding 0.1g dopamine hydrochloride, stirring and reacting for 6h at room temperature; washing the obtained product with deionized water and ethanol for 3 times respectively, filtering, and drying to obtain polydopamine-coated ferric oxide compound (Fe) 2 O 3 @PDA-2);
S3, calcining to prepare the composite wave-absorbing material: mixing Fe 2 O 3 Putting the @ PDA-2 compound powder into a tubular furnace, and calcining at 500 ℃ for 6h in an inert atmosphere to obtain the magnetic nanoparticle coated microcapsule-like carbon-based composite material (Fe) 3 O 4 @C-2)。
Example 3: a preparation method of a magnetic nanoparticle coated microcapsule-shaped carbon-based composite material comprises the following steps:
s1, preparing a microcapsule template core: stirring 250mL of ferric trichloride with crystal water at the concentration of 2mol/L for 30min at the temperature of 75 ℃, dropwise adding 250mL of sodium hydroxide aqueous solution at the concentration of 6mol/L, continuously stirring for 30min, then adding 25mL of sodium sulfate aqueous solution at the concentration of 1mol/L, uniformly mixing, injecting the mixed solution into a reaction kettle, putting the reaction kettle into an oven for reaction at the temperature of 120 ℃ for 48h, washing the obtained product with deionized water to be neutral, performing suction filtration, and freeze-drying to obtain microcapsule-shaped ferric oxide (Fe) 2 O 3 -3) a template core;
s2, carrying out chemical polymerization coating on the surface of the template core: 0.1g of Fe 2 O 3 -3, uniformly dispersing the template core in a tris (hydroxymethyl) aminomethane aqueous solution with the pH =8.5, adding 0.2g of dopamine hydrochloride, stirring and reacting for 6h at room temperature; washing the obtained product with deionized water and ethanol for 3 times respectively, filtering, and drying to obtain polydopamine-coated ferric oxide compound (Fe) 2 O 3 @PDA-3);
S3, calcining to prepare the composite wave-absorbing material: mixing Fe 2 O 3 The @ PDA-3 composite powder is placed in a tube furnace and subjected to high-temperature calcination in an inert atmosphereThe calcining temperature is 600 ℃, the calcining time is 2h, and the magnetic nano particle coated microcapsule carbon-based composite material (Fe) is obtained 3 O 4 @C-3)。
Example 4: a preparation method of a magnetic nanoparticle coated microcapsule-shaped carbon-based composite material comprises the following steps:
s1, preparing a microcapsule template core: stirring 250mL of ferric trichloride with crystal water at the concentration of 2mol/L for 30min at the temperature of 75 ℃, dropwise adding 250mL of sodium hydroxide aqueous solution at the concentration of 4mol/L, continuously stirring for 30min, then adding 25mL of sodium sulfate aqueous solution at the concentration of 0.8mol/L, uniformly mixing, injecting the mixed solution into a reaction kettle, putting the reaction kettle into an oven for reaction at the temperature of 100 ℃ for 60h, washing the obtained product with deionized water to be neutral, performing suction filtration, and freeze drying to obtain microcapsule-shaped ferric oxide (Fe) 2 O 3 -4) a template core;
s2, carrying out chemical polymerization coating on the surface of the template core: 0.1g of Fe 2 O 3 -4, uniformly dispersing template cores in a tris (hydroxymethyl) aminomethane aqueous solution with the pH =8.5, adding 0.1g dopamine hydrochloride, stirring and reacting for 6h at room temperature; washing the obtained product with deionized water and ethanol for 3 times respectively, filtering, and drying to obtain polydopamine-coated ferric oxide compound (Fe) 2 O 3 @PDA-4);
S3, calcining to prepare the composite wave-absorbing material: mixing Fe 2 O 3 Putting the @ PDA-4 compound powder into a tubular furnace, and calcining at 800 ℃ for 3h in an inert atmosphere to obtain the magnetic nanoparticle coated microcapsule-like carbon-based composite material (Fe) 3 O 4 @C-4)。
Example 5: a preparation method of a magnetic nanoparticle coated microcapsule-shaped carbon-based composite material comprises the following steps:
s1, preparing a microcapsule template core: stirring 250mL of ferric trichloride with crystal water at the concentration of 2mol/L for 30min at the temperature of 75 ℃, dropwise adding 250mL of sodium hydroxide aqueous solution at the concentration of 3mol/L, continuously stirring for 30min, then adding 25mL of sodium sulfate aqueous solution at the concentration of 0.5mol/L, uniformly mixing,after being uniformly mixed, the mixed solution is injected into a reaction kettle and is put into a drying oven for reaction, the temperature of the drying oven is 120 ℃, the reaction time is 60 hours, the obtained product is washed to be neutral by deionized water, and the microcapsule-shaped ferric oxide (Fe) is obtained after suction filtration and freeze drying 2 O 3 -5) a template core;
s2, carrying out chemical polymerization coating on the surface of the template core: 0.1g of Fe 2 O 3 -5, uniformly dispersing the template core in a tris (hydroxymethyl) aminomethane aqueous solution with the pH =8.5, adding 0.05g of dopamine hydrochloride, stirring and reacting for 6h at room temperature; washing the obtained product with deionized water and ethanol for 3 times respectively, filtering, and drying to obtain polydopamine-coated ferric oxide compound (Fe) 2 O 3 @PDA-5);
S3, calcining to prepare the composite wave-absorbing material: mixing Fe 2 O 3 Putting the @ PDA-5 composite powder into a tubular furnace, and calcining at 900 ℃ for 4h in an inert atmosphere to obtain the magnetic nanoparticle coated microcapsule-like carbon-based composite material (Fe) 3 O 4 @C-5)。
Example 6: the invention provides a preparation method of a magnetic nanoparticle coated microcapsule-shaped carbon-based composite material, which comprises the following steps:
s1, preparing a microcapsule template core: stirring 250mL of ferric trichloride with crystal water at the concentration of 2mol/L for 30min at the temperature of 75 ℃, dropwise adding 250mL of sodium hydroxide aqueous solution at the concentration of 5.4mol/L, continuously stirring for 30min, then adding 25mL of sodium sulfate aqueous solution at the concentration of 0.6mol/L, uniformly mixing, injecting the mixed solution into a reaction kettle, putting the reaction kettle into an oven for reaction, wherein the oven temperature is 110 ℃, the reaction time is 72h, washing the obtained product with deionized water to be neutral, performing suction filtration, and freeze drying to obtain the microcapsule-shaped ferric oxide (Fe) 2 O 3 -6) a template core;
s2, performing chemical polymerization coating on the surface of the template core: 0.1g of Fe 2 O 3 -1, uniformly dispersing template cores in a tris (hydroxymethyl) aminomethane aqueous solution with the pH =8.5, adding 0.15g dopamine hydrochloride, stirring and reacting for 6h at room temperature; washing the obtained product with deionized water and ethanol for 3 times respectively, filtering, and oven dryingThen obtaining a polydopamine-coated ferric oxide compound (Fe) 2 O 3 @PDA-6);
S3, calcining to prepare the composite wave-absorbing material: mixing Fe 2 O 3 Putting the @ PDA-6 composite powder into a tubular furnace, and calcining at the high temperature of 750 ℃ for 4h in an inert atmosphere to obtain the magnetic nanoparticle coated microcapsule-like carbon-based composite material (Fe) 3 O 4 @C-6)。
In the process of preparing the microcapsule-shaped template core, the molar concentrations of a sodium hydroxide aqueous solution and a sodium sulfate aqueous solution have large influence on the shape of the template core, so that the solution molar concentration needs to be strictly controlled, the molar concentration of the sodium hydroxide aqueous solution is controlled within a range of 3 to 6mol/L, and the molar concentration of the sodium sulfate aqueous solution is controlled within a range of 0.5 to 1mol/L.
FIG. 5 shows different Fe values obtained in examples 1 to 6 3 O 4 According to the reflection loss curve of the @ C composite material under the same matching thickness, the wave-absorbing performance of the composite material obtained under the conditions of different proportions, particularly effective absorption frequency band and minimum reflection loss value, can be greatly different, so that the wave-absorbing performance of the composite material can be regulated and controlled by simply controlling the metal particle precursor, dopamine hydrochloride and high-temperature calcination treatment temperature, and the electromagnetic parameters and the electromagnetic wave absorption capacity of the product can be controlled and adjusted.
The mass ratio of the microcapsule-shaped ferric oxide core to the dopamine hydrochloride in the method and the high-temperature calcination treatment temperature in the later period not only influence the finally obtained Fe 3 O 4 The dielectric/magnetic properties of the @ C composite material also affect the attenuation performance and matching performance of the composite material, and further affect the wave-absorbing performance of the composite material.
According to the method, the microcapsule-shaped ferric oxide core is synthesized, polydopamine is coated on the surface of the microcapsule-shaped ferric oxide core by taking the microcapsule-shaped ferric oxide core as a template, and the mixture coated with the polydopamine is calcined at high temperature to prepare the magnetic nanoparticle-coated microcapsule-shaped carbon-based composite wave-absorbing material.
The above description is only for the purpose of illustrating the technical solutions of the present invention and not for the purpose of limiting the same, and other modifications or equivalent substitutions made by those skilled in the art to the technical solutions of the present invention should be covered within the scope of the claims of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. A preparation method of a magnetic nanoparticle coated microcapsule-shaped carbon-based composite material is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing a microcapsule template core: stirring ferric iron metal salt with the concentration of 2mol/L for 30min at the temperature of 75 ℃, dropwise adding sodium hydroxide aqueous solution with the concentration of 3-6 mol/L, continuously stirring for 30min, then adding sodium sulfate aqueous solution with the concentration of 0.5-1mol/L, uniformly mixing, injecting the mixed solution into a reaction kettle, putting the reaction kettle into an oven for reaction, washing the obtained product with deionized water to be neutral, performing suction filtration, and performing freeze drying to obtain a microcapsule-shaped ferric oxide template core;
s2, carrying out chemical polymerization coating on the surface of the template core: uniformly dispersing the microcapsule-shaped ferric oxide template core prepared in the step S1 into a trihydroxymethyl aminomethane aqueous solution with the pH =8.5, adding dopamine hydrochloride, stirring and reacting for 6h at room temperature, wherein the mass ratio of the ferric oxide template core to the dopamine hydrochloride is (1); washing the obtained product with deionized water and ethanol for 3 times respectively, performing suction filtration, and drying to obtain a polydopamine-coated ferric oxide compound;
s3, calcining to prepare the composite wave-absorbing material: and (3) placing the polydopamine coated ferric oxide compound powder prepared in the step (S2) in a tubular furnace, and calcining at a high temperature of 500-900 ℃ for 2-6 h in an inert atmosphere to obtain the magnetic nanoparticle coated microcapsule-shaped carbon-based composite material.
2. The method for preparing the magnetic nanoparticle-coated microcapsule-like carbon-based composite material according to claim 1, wherein: in the step S1, the molar concentration of the sodium hydroxide aqueous solution is preferably 5.4mol/L, and the molar concentration of the sodium sulfate aqueous solution is preferably 0.6mol/L.
3. The method for preparing the magnetic nanoparticle-coated microcapsule-like carbon-based composite material according to claim 1, wherein: in the step S1, the ferric iron metal salt is ferric trichloride with crystal water.
4. The method for preparing the magnetic nanoparticle-coated microcapsule-like carbon-based composite material according to claim 1, wherein: in the step S1, the temperature of an oven is 100 to 120 ℃, the reaction time is 48 to 96h, the optimal temperature is 110 ℃, and the optimal reaction time is 72h.
5. The method for preparing the magnetic nanoparticle-coated microcapsule-like carbon-based composite material according to claim 1, wherein: in the step S2, preferably, the mass ratio of the ferric oxide template core to the dopamine hydrochloride is 1.
6. The method for preparing the magnetic nanoparticle-coated microcapsule-like carbon-based composite material according to claim 1, wherein: in the step S2, preferably, the calcination temperature is 750 ℃ and the calcination time is 4 hours.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104984693A (en) * | 2015-07-24 | 2015-10-21 | 扬州大学 | Preparation method of nanometer magnetism capsule |
CN109825252A (en) * | 2019-03-04 | 2019-05-31 | 安徽理工大学 | Core-shell structure Fe3O4@C@MoS2The preparation and its application of composite material |
CN111117564A (en) * | 2019-12-03 | 2020-05-08 | 安徽理工大学 | Yolk-eggshell type magnetic carbon composite material, preparation method and application |
CN114824202A (en) * | 2022-04-12 | 2022-07-29 | 南京师范大学 | FeS with multi-core shell structure 2 Preparation method and application of @ C nanocapsule material |
-
2022
- 2022-10-27 CN CN202211327043.1A patent/CN115636443A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104984693A (en) * | 2015-07-24 | 2015-10-21 | 扬州大学 | Preparation method of nanometer magnetism capsule |
CN109825252A (en) * | 2019-03-04 | 2019-05-31 | 安徽理工大学 | Core-shell structure Fe3O4@C@MoS2The preparation and its application of composite material |
CN111117564A (en) * | 2019-12-03 | 2020-05-08 | 安徽理工大学 | Yolk-eggshell type magnetic carbon composite material, preparation method and application |
CN114824202A (en) * | 2022-04-12 | 2022-07-29 | 南京师范大学 | FeS with multi-core shell structure 2 Preparation method and application of @ C nanocapsule material |
Non-Patent Citations (1)
Title |
---|
周影影: "磁性吸波材料", vol. 1, 陕西科学技术出版社, pages: 78 - 79 * |
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