CN113429933A - Ferroferric oxide/biomass porous carbon composite wave-absorbing material and preparation method thereof - Google Patents
Ferroferric oxide/biomass porous carbon composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ferroferric oxide/biomass porous carbon composite wave-absorbing material and a preparation method thereof, belonging to the field of wave-absorbing materials. The preparation method comprises the following steps: cleaning and drying a biomass carbon source, and soaking the dried biomass carbon source in an iron source solution to absorb iron ions; and cleaning and drying the soaked biomass carbon source, and then calcining to prepare the ferroferric oxide/biomass porous carbon composite wave-absorbing material. The invention effectively overcomes the defects of easy agglomeration, poor temperature adaptability and poor low-frequency absorption performance of the existing material. The ferroferric oxide/biomass porous carbon composite wave-absorbing material prepared by the method has low density, less agglomeration phenomenon and obviously improved wave-absorbing performance.
Description
Technical Field
The invention belongs to the field of wave-absorbing materials, and relates to a ferroferric oxide/biomass porous carbon composite wave-absorbing material and a preparation method thereof.
Background
The ferrite material is used as an important absorbent of electromagnetic waves, is a double-composite dielectric material, has both magnetic and dielectric properties, so that the ferrite material has good wave-absorbing property, low cost and small volume, and has not only magnetic absorption but also electric absorption on the electromagnetic waves in the aspect of impedance matching; in terms of attenuation matching, magnetic loss and electric loss are also sources of loss of electromagnetic waves, and the combination of the two can enable the electromagnetic waves to obtain maximum absorption and loss. The ferrite material also avoids the disadvantages such as high density, narrow absorption band and poor high temperature resistance.
Fe3O4The powder electromagnetic wave absorbent has the advantages of wide raw materials, easy preparation, no toxicity and the like, but is easy to agglomerate and poor in temperature adaptation. The nano ferroferric oxide is an electromagnetic wave absorbing material with excellent performance, but the application of the nano ferroferric oxide is severely limited due to the narrow absorption band and easy agglomeration.
Fe3O4Is an electromagnetic wave absorbent with great potential in the prior magnetic material, Fe3O4In the presence of Fe2+And Fe3+The free electrons in the material are easy to transit between different ions, so that the material has the semiconductor property and certain conductivity, and is a double-loss dielectric material. However Fe3O4As one of the research hotspots of the electromagnetic wave absorbing material, it is still difficult to satisfy the performance requirements of thin thickness, light weight, wide frequency band and strong absorption of the electromagnetic wave absorbing material, and the material has a certain electromagnetic wave absorbing effect only in the low frequency range, so Fe3O4It still cannot be directly used as an electromagnetic wave absorbing material.
The biomass carbon refers to a material prepared by removing non-carbon elements contained in the material itself through high-temperature sintering with organic compounds naturally occurring in nature, such as plants and the like. The material has the characteristics of wide and easily available raw materials, low cost, large specific surface area, high porosity, stable performance, environmental friendliness and the like, and becomes a research hotspot of the current wave-absorbing material. Recent researches find that the biomass carbon material has a unique microstructure, and a plurality of microscopic pore canals in the biomass carbon material can not only reduce the density and the conductivity of the material, but also be beneficial to improving the impedance matching performance of the material, so that electromagnetic waves enter the material as much as possible to generate multiple scattering and reflection, and the electromagnetic waves are consumed. In addition, the surface of the biomass carbon contains a large number of oxygen-containing functional groups, so that more electron dipole polarization can be generated, and the biomass carbon is favorable for being compounded with other materials.
The loss mechanism of the biomass carbon material is limited to unidirectional dielectric loss and is not enough to obtain proper impedance matching. In this case, a large portion of the electromagnetic wave is easily reflected from the absorber surface, rather than being attenuated. Therefore, impedance matching should be prioritized. The introduction of magnetic materials into the carbon system is an effective method for adjusting the complex dielectric constant and complex permeability of the absorber, so that impedance matching can be enhanced, and the absorption performance can be improved. With the addition of Fe, the magnetic loss of the composite material is improved, but too much Fe causes impedance mismatch of the composite material.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide ferroferric oxide/biomass porous carbon (Fe)3O4the/BPC) composite wave-absorbing material and the preparation method thereof solve the defects of easy agglomeration, poor temperature adaptability and poor low-frequency absorption performance of the existing material. Fe prepared by the invention3O4the/BPC composite wave-absorbing material has low density, less agglomeration and obviously improved wave-absorbing performance.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses a preparation method of a ferroferric oxide/biomass porous carbon composite wave-absorbing material, which comprises the following steps:
cleaning and drying a biomass carbon source, and soaking the dried biomass carbon source in an iron source solution to absorb iron ions; and cleaning and drying the soaked biomass carbon source, and then calcining to prepare the ferroferric oxide/biomass porous carbon composite wave-absorbing material.
Preferably, the biomass carbon source is agaric.
Preferably, the washing operation of the biomass carbon source comprises: ultrasonically cleaning a biomass carbon source in ethanol; the drying operation of the biomass carbon source comprises the following steps: drying at 60 deg.C for 2 h.
Preferably, the iron source solution is an iron nitrate solution, an iron sulfate solution, an iron chloride solution or an iron acetate solution.
Preferably, the concentration of the iron source solution is 0.2-2 mol/L.
Preferably, the feeding ratio of the biomass carbon source to the iron source solution is 10 g: 100 mL.
Preferably, the soaking temperature is 60-80 ℃, and the soaking time is 6-18 h.
Preferably, the operating parameters of the calcination treatment include: calcining for 2h at the temperature of 400-800 ℃ under vacuum.
The invention discloses a ferroferric oxide/biomass porous carbon composite wave-absorbing material prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of a ferroferric oxide/biomass porous carbon composite wave-absorbing material, which takes a biomass material as a carbon source and can utilize a pore structure in biomass carbon to subsequently generate Fe3O4The Fe-containing composite material is doped into the pore channel, and Fe can be prepared by adopting a simple process by soaking a biomass carbon source into an iron source solution for adsorption treatment3O4A composite material doped into a biomass carbon source. Therefore, the preparation method has the advantages of simple process operation and wide application range, and can effectively solve the problem of material agglomeration.
Furthermore, by selecting the agaric as the biomass carbon source and utilizing the extremely strong water absorption capacity of the agaric, in the specific embodiment of the invention, the volume of the dry agaric can be expanded to more than twenty times of the original volume after water absorption,and the water absorption and dehydration process can be circulated for many times, and the agaric structure has good stability. In addition, the agaric has strong adsorption capacity to metal salt solution, and metal salt ions can be uniformly dispersed in cells and gaps among tissues of the agaric. Thereby effectively avoiding agglomeration and realizing Fe3O4And (4) adsorption of magnetic particles.
The invention discloses a ferroferric oxide/biomass porous carbon composite wave-absorbing material prepared by the preparation method, wherein a biomass carbon source has rich pore structure, and Fe3O4Magnetic particles are embedded into the pore channels of the biomass carbon and attached to the surface of the biomass carbon source, and Fe is doped in the biomass carbon source material3O4The nano particles can reduce the real part epsilon 'and the imaginary part epsilon' of the dielectric constant, increase the real part mu 'and the imaginary part mu' of the magnetic conductivity and increase the loss tangent value tan delta; doping Fe in biomass carbon source material3O4The reflectivity loss of the composite material of the nano particles is reduced, and the maximum absorption peak moves to low frequency, which means that the wave absorbing capacity is improved. Therefore, the invention can obviously improve the wave-absorbing performance of the prepared material while reducing the agglomeration phenomenon.
Drawings
FIG. 1 is a SEM photograph of a product prepared in example 5 of the present invention;
FIG. 2 is a XRD test result of the product prepared in example 5 of the present invention;
FIG. 3 is a wave-absorbing property test result chart of the finished product prepared in example 5 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention adopts a direct carbonization method to prepare the embedded Fe3O4The biomass carbon magnetic wave-absorbing material of the magnetic particles is the ferroferric oxide/biomass porous carbon (Fe)3O4/BPC) (BPC, bioglass porous carbon) composite wave-absorbing material. Said Fe3O4The preparation method of the/BPC composite wave-absorbing material specifically comprises the following steps:
(1) ultrasonically cleaning a biomass carbon source in ethanol, and drying in an oven after cleaning.
(2) And (3) immersing the dried biomass carbon source into a ferric nitrate/ferric sulfate/ferric chloride/ferric acetate solution, and putting the biomass carbon source into an oven for a period of time to enable the biomass carbon source to fully absorb iron ions.
(3) And taking out the soaked biomass carbon source, ultrasonically cleaning, and drying in an oven.
(4) Calcining the soaked and dried biomass carbon source serving as a precursor in a horizontal vacuum tubular furnace under vacuum to obtain the composite material of ferroferric oxide and biomass porous carbon, namely Fe3O4the/BPC composite wave-absorbing material.
Preferably, the biomass carbon source in the step (1) is agaric, the ultrasonic cleaning time is 1 hour, and the drying temperature of the oven is 60 ℃ for drying for 2 hours.
Preferably, 10g of biomass carbon source is put into the step (2), and the concentration of the ferric nitrate/ferric sulfate/ferric chloride/ferric acetate solution is 100ml0.2-2 mol/L.
Preferably, in the step (2), the dried biomass carbon source is soaked in a beaker filled with ferric nitrate/ferric sulfate/ferric chloride/ferric acetate solution, and the whole beaker system is sealed by a preservative film before being placed in an oven, so that volatilization is avoided, and the agaric can better absorb iron ions.
Preferably, the drying temperature of the oven in the step (2) is 60-80 ℃, and the standing time is 6-18 h.
Preferably, the ultrasonic cleaning time in the step (3) is 30min, and the drying temperature of the oven is 60 ℃ for drying for 36 h.
Preferably, the tubular furnace in the step (4) is calcined for 2 hours at the temperature rise rate of 5 ℃/min to 400-800 ℃ under vacuum to obtain the composite material (Fe) of the ferroferric oxide and the biomass porous carbon3O4/BPC)。
The present invention is described in further detail below with reference to specific examples:
example 1
(1) Ultrasonically cleaning dried Auricularia in ethanol for 1 hr, and drying in oven at 60 deg.C for 2 hr.
(2) 10g of agaric is immersed into a beaker containing 100ml of 0.2mol/L ferric nitrate solution, the beaker is sealed by a preservative film and then is placed into an oven at 60 ℃ for 6 hours to fully absorb iron ions.
(3) Taking out the soaked Auricularia, ultrasonically cleaning for 30min, and drying in an oven at 60 deg.C for 36 h.
(4) Calcining the soaked and dried agaric serving as a precursor for 2 hours at the temperature rise rate of 5 ℃/min to 400 ℃ in vacuum to obtain the ferroferric oxide and biomass porous carbon composite material (Fe)3O4/BPC), i.e. Fe3O4the/BPC composite wave-absorbing material.
Example 2
(1) Ultrasonically cleaning dried Auricularia in ethanol for 1 hr, and drying in oven at 60 deg.C for 2 hr.
(2) 10g of agaric is immersed into a beaker containing 100mL of 2mol/L ferric nitrate solution, the beaker is sealed by a preservative film and then is placed into an oven at 60 ℃ for 6 hours to fully absorb iron ions.
(3) Taking out the soaked Auricularia, ultrasonically cleaning for 30min, and drying in an oven at 60 deg.C for 36 h.
(4) Calcining the soaked and dried agaric serving as a precursor for 2 hours at the temperature rise rate of 5 ℃/min to 600 ℃ in vacuum to obtain the ferroferric oxide and biomass porous carbon composite material (Fe)3O4/BPC), i.e. Fe3O4the/BPC composite wave-absorbing material.
Example 3
(1) Ultrasonically cleaning dried Auricularia in ethanol for 1 hr, and drying in oven at 60 deg.C for 2 hr.
(2) 10g of agaric is immersed into a beaker containing 100ml of 0.2mol/L ferric nitrate solution, the beaker is sealed by a preservative film and then is placed into an oven at 60 ℃ for 6 hours to fully absorb iron ions.
(3) Taking out the soaked Auricularia, ultrasonically cleaning for 30min, and drying in an oven at 60 deg.C for 36 h.
(4) Calcining the soaked and dried agaric serving as a precursor for 2 hours at the temperature rise rate of 5 ℃/min to 800 ℃ in vacuum to obtain the ferroferric oxide and biomass porous carbon composite material (Fe)3O4/BPC), i.e. Fe3O4the/BPC composite wave-absorbing material.
Example 4
(1) Ultrasonically cleaning dried Auricularia in ethanol for 1 hr, and drying in oven at 60 deg.C for 2 hr.
(2) 10g of agaric is immersed into a beaker containing 100mL of 1mol/L ferric nitrate solution, the beaker is sealed by a preservative film and then is placed into an oven at 60 ℃ for 6 hours to fully absorb iron ions.
(3) Taking out the soaked Auricularia, ultrasonically cleaning for 30min, and drying in an oven at 60 deg.C for 36 h.
(4) Calcining the soaked and dried agaric serving as a precursor for 2 hours at the temperature rise rate of 5 ℃/min to 800 ℃ in vacuum to obtain the ferroferric oxide and biomass porous carbon composite material (Fe)3O4/BPC), i.e. Fe3O4the/BPC composite wave-absorbing material.
Example 5
(1) Ultrasonically cleaning dried Auricularia in ethanol for 1 hr, and drying in oven at 60 deg.C for 2 hr.
(2) 10g of agaric is immersed into a beaker containing 100mL of 2mol/L ferric nitrate solution, the beaker is sealed by a preservative film and then is placed into an oven at 60 ℃ for 6 hours to fully absorb iron ions.
(3) Taking out the soaked Auricularia, ultrasonically cleaning for 30min, and drying in an oven at 60 deg.C for 36 h.
(4) Calcining the soaked and dried agaric serving as a precursor for 2 hours at the temperature rise rate of 5 ℃/min to 800 ℃ in vacuum to obtain the ferroferric oxide and biomass porous carbon composite material (Fe)3O4/BPC), i.e. Fe3O4the/BPC composite wave-absorbing material.
Example 6
(1) Ultrasonically cleaning dried Auricularia in ethanol for 1 hr, and drying in oven at 60 deg.C for 2 hr.
(2) 10g of agaric is immersed in a beaker containing 100ml of 1.5 mol/L ferric sulfate solution, the beaker is sealed by a preservative film and then is placed in an oven at 70 ℃ for 18 hours to fully absorb iron ions.
(3) Taking out the soaked Auricularia, ultrasonically cleaning for 30min, and drying in an oven at 60 deg.C for 36 h.
(4) Calcining the soaked and dried agaric serving as a precursor for 2 hours at the temperature rise rate of 5 ℃/min to 500 ℃ in vacuum to obtain the ferroferric oxide and biomass porous carbon composite material (Fe)3O4/BPC), i.e. Fe3O4the/BPC composite wave-absorbing material.
Example 7
(1) Ultrasonically cleaning dried Auricularia in ethanol for 1 hr, and drying in oven at 60 deg.C for 2 hr.
(2) 10g of agaric is immersed into a beaker containing 100ml of 0.5 mol/L ferric chloride solution, the beaker is sealed by a preservative film and then is placed into an oven at 80 ℃ for 18 hours to fully absorb iron ions.
(3) Taking out the soaked Auricularia, ultrasonically cleaning for 30min, and drying in an oven at 60 deg.C for 36 h.
(4) Calcining the soaked and dried agaric as a precursor for 2 hours at the temperature rising rate of 5 ℃/min to 700 ℃ in vacuum to obtain the agaricComposite material (Fe) of ferroferric oxide and biomass porous carbon3O4/BPC), i.e. Fe3O4the/BPC composite wave-absorbing material.
Example 8
(1) Ultrasonically cleaning dried Auricularia in ethanol for 1 hr, and drying in oven at 60 deg.C for 2 hr.
(2) 10g of agaric is immersed into a beaker containing 100ml of 1.1 mol/L ferric acetate solution, the beaker is sealed by a preservative film and then is placed into an oven at 65 ℃ for 18 hours to fully absorb iron ions.
(3) Taking out the soaked Auricularia, ultrasonically cleaning for 30min, and drying in an oven at 60 deg.C for 36 h.
(4) Calcining the soaked and dried agaric serving as a precursor for 2 hours at the temperature rise rate of 5 ℃/min to 550 ℃ in vacuum to obtain the ferroferric oxide and biomass porous carbon composite material (Fe)3O4/BPC), i.e. Fe3O4the/BPC composite wave-absorbing material.
Example 9
(1) Ultrasonically cleaning dried Auricularia in ethanol for 1 hr, and drying in oven at 60 deg.C for 2 hr.
(2) 10g of agaric is immersed in a beaker containing 100ml of 1.8 mol/L ferric chloride solution, the beaker is sealed by a preservative film and then is placed in an oven at the temperature of 75 ℃ for 6 hours to fully absorb iron ions.
(3) Taking out the soaked Auricularia, ultrasonically cleaning for 30min, and drying in an oven at 60 deg.C for 36 h.
(4) Calcining the soaked and dried agaric serving as a precursor for 2 hours at the temperature rise rate of 5 ℃/min to 680 ℃ in vacuum to obtain the ferroferric oxide and biomass porous carbon composite material (Fe)3O4/BPC), i.e. Fe3O4the/BPC composite wave-absorbing material.
The invention is described in further detail below with reference to the accompanying drawings:
the biomass carbon source obtained by carbonization as shown in figure 1 has rich pore structure, Fe3O4The uniform embedding on the biomass carbon source can be seen, and uniform Fe is also embedded in the pore channel structure3O4Magnetic particles.
As shown in figure 2, the ferroferric oxide/biomass porous carbon composite wave-absorbing material has diffraction peaks at 30.1 degrees, 35.3 degrees, 57.07 degrees and 62.5 degrees, which are similar to those of Fe3O4The standard card of (JCPDS card; 19-0629) was identical, which shows that Fe was successfully synthesized3O4Magnetic particles. Diffraction peaks at 45 ° and 65 ° indicate the generation of Fe phase, and the sharper peaks indicate better crystallinity.
As shown in FIG. 3, the maximum absorption peak value of the ferroferric oxide/biomass porous carbon composite wave-absorbing material is-30.4 dB, the maximum absorption bandwidth is 2.45GHz, and the thickness at the moment is 2.06 mm.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. A preparation method of a ferroferric oxide/biomass porous carbon composite wave-absorbing material is characterized by comprising the following steps:
cleaning and drying a biomass carbon source, and soaking the dried biomass carbon source in an iron source solution to absorb iron ions; and cleaning and drying the soaked biomass carbon source, and then calcining to prepare the ferroferric oxide/biomass porous carbon composite wave-absorbing material.
2. The preparation method of the ferroferric oxide/biomass porous carbon composite wave-absorbing material according to claim 1, characterized in that the biomass carbon source is agaric.
3. The preparation method of the ferroferric oxide/biomass porous carbon composite wave-absorbing material according to claim 1, characterized in that the operation of cleaning the biomass carbon source comprises: ultrasonically cleaning a biomass carbon source in ethanol;
the drying operation of the biomass carbon source comprises the following steps: drying at 60 deg.C for 2 h.
4. The preparation method of the ferroferric oxide/biomass porous carbon composite wave-absorbing material according to claim 1, characterized in that the iron source solution is ferric nitrate solution, ferric sulfate solution, ferric chloride solution or ferric acetate solution.
5. The preparation method of the ferroferric oxide/biomass porous carbon composite wave-absorbing material according to claim 1, characterized in that the concentration of the iron source solution is 0.2-2 mol/L.
6. The preparation method of the ferroferric oxide/biomass porous carbon composite wave-absorbing material according to claim 1, characterized in that the feeding ratio of a biomass carbon source to an iron source solution is 10 g: 100 mL.
7. The preparation method of the ferroferric oxide/biomass porous carbon composite wave-absorbing material according to claim 1, characterized in that the soaking temperature is 60-80 ℃ and the soaking time is 6-18 h.
8. The preparation method of the ferroferric oxide/biomass porous carbon composite wave-absorbing material according to claim 1, characterized in that the operational parameters of the calcination treatment include: calcining for 2h at the temperature of 400-800 ℃ under vacuum.
9. The ferroferric oxide/biomass porous carbon composite wave-absorbing material prepared by the preparation method of any one of claims 1 to 8.
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| CN115851227A (en) * | 2022-12-15 | 2023-03-28 | 青岛科技大学 | PC/Fe 3 O 4 @ PDA hybrid nano composite wave-absorbing material and preparation method thereof |
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| CN113753894A (en) * | 2021-09-30 | 2021-12-07 | 山西华青环保股份有限公司 | Preparation method of ferroferric oxide loaded active carbon |
| CN115851227A (en) * | 2022-12-15 | 2023-03-28 | 青岛科技大学 | PC/Fe 3 O 4 @ PDA hybrid nano composite wave-absorbing material and preparation method thereof |
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