CN114108135A - Carbon/manganese oxide/cobalt nano composite fiber and preparation method and application thereof - Google Patents
Carbon/manganese oxide/cobalt nano composite fiber and preparation method and application thereof Download PDFInfo
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- CN114108135A CN114108135A CN202111273402.5A CN202111273402A CN114108135A CN 114108135 A CN114108135 A CN 114108135A CN 202111273402 A CN202111273402 A CN 202111273402A CN 114108135 A CN114108135 A CN 114108135A
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- cobalt
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- manganese oxide
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
Abstract
The invention discloses a carbon/manganese oxide/cobalt nano composite fiber and a preparation method and application thereof. The manganese oxide nanoparticles are introduced, and have low conductivity and low dielectric constant, the low conductivity can inhibit the generation of eddy current, and the low dielectric constant enables the manganese oxide nanoparticles to have the advantages of conveniently regulating and controlling electromagnetic parameters and optimizing impedance matching; due to the two factors, the manganese oxide is beneficial to the entering of electromagnetic waves, and different dissipation mechanisms can be fully utilized at the same time, so that better absorption performance is obtained.
Description
Technical Field
The invention belongs to the technical field of electromagnetic wave absorbing materials, and particularly relates to a carbon/manganese oxide/cobalt nano composite fiber and a preparation method and application thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
The basic working principle of the wave-absorbing material is to convert electromagnetic energy in incident electromagnetic waves into heat energy or energy in other forms so as to achieve the purpose of effectively attenuating the electromagnetic waves. According to the transmission line theory, the wave-absorbing material not only needs stronger loss capacity, but also needs better impedance matching so as to enable the electromagnetic wave to be incident into the material as much as possible and to be in full contact with the material. The conditions required for stronger losses and better matching tend to be counter-productive.
The first wave-absorbing materials studied were magnetic metals (including iron, cobalt, nickel, ferrites, and related composites). The material has strong attenuation characteristic and is widely applied to the field of electromagnetic wave absorption. However, since magnetic metals generally have high density and poor corrosion resistance, they are difficult to be applied to environments of high temperature and high pressure or strong acid and strong base. Moreover, the single magnetic material component has fewer loss ways for incident electromagnetic waves, and the requirement of the novel wave-absorbing material is difficult to meet. In order to expand the application range of the wave-absorbing material and increase the loss path, the prior art uses carbon materials and magnetic metals for compounding. The carbon material is widely applied to adjusting the electromagnetic parameters of the wave-absorbing material due to the characteristics of large specific surface area, low density, adjustable conductivity, good chemical stability and the like. Compared with a single carbon material or a single magnetic component, the carbon-based composite material has better loss capacity and larger effective absorption bandwidth, and the wave-absorbing performance of the whole material is improved. However, the inventors found that the recombination of the carbon material and the magnetic metal results in poor impedance matching, and that the surface of the material inevitably reflects electromagnetic waves, thereby being disadvantageous to the effective absorption of the electromagnetic waves.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a carbon/manganese oxide/cobalt nano composite fiber and a preparation method and application thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
in a first aspect, the present invention provides a carbon/manganese oxide/cobalt nanocomposite fiber comprising a carbon fiber, cobalt nanoparticles attached to the surface of the carbon fiber, and manganese oxide nanoparticles.
In a second aspect, the invention provides a preparation method of the carbon/manganese oxide/cobalt nano composite fiber, which comprises the following steps:
dissolving a cobalt source, a manganese source and a carbon source in an organic solvent to form a spinning solution, spinning the spinning solution to prepare a precursor, and drying, pre-oxidizing and thermally treating the precursor to obtain the catalyst.
In a third aspect, the invention provides an application of the carbon/manganese oxide/cobalt nano composite fiber as an electromagnetic wave absorbing material, especially an application as a 2-18GHz electromagnetic wave absorbing material.
The beneficial effects achieved by one or more of the embodiments of the invention described above are as follows:
1. the manganese oxide nanoparticles are introduced, and have low conductivity and low dielectric constant, the low conductivity can inhibit the generation of eddy current, and the low dielectric constant enables the manganese oxide nanoparticles to have the advantages of conveniently regulating and controlling electromagnetic parameters and optimizing impedance matching; due to the two factors, the manganese oxide is beneficial to the entering of electromagnetic waves, and different dissipation mechanisms can be fully utilized at the same time, so that better absorption performance is obtained.
The one-dimensional structure of the carbon fiber not only has larger surface area, but also is beneficial to forming a conductive network, thereby generating micro current and increasing the conductance loss when electromagnetic waves are incident. The uniformly embedded cobalt nanoparticles and manganese oxide nanoparticles also provide advantages for multiple scattering of electromagnetic waves. In addition, the large number of interfaces between the nanoparticles and the carbon fibers provides a large number of sites for interface polarization loss under an electromagnetic field, further increasing dielectric loss. In combination with the introduced magnetic loss mechanism, the carbon/manganese oxide/cobalt nanocomposite fibers thus exhibit excellent microwave absorption properties.
2. The carbon/manganese oxide/cobalt nano composite fiber material is obtained by electrostatic spinning and heat treatment in hydrogen atmosphere, the parameters in the preparation process are controllable, the process is simple, the cost is low, the carbon/manganese oxide/cobalt nano composite fiber material is suitable for industrial production, the preparation efficiency of the composite material is high, and the material utilization rate is high.
The macro and micro appearance, electromagnetic parameters, wave-absorbing performance and the like of the prepared carbon/manganese oxide/cobalt nano composite fiber material can be easily adjusted by adjusting parameters in the preparation process. The method is beneficial to preparing the wave-absorbing material suitable for different environments and widening the use scene of the material.
3. The precursor is prepared by electrostatic spinning, and then the wave-absorbing material is prepared by heat treatment, so that the prepared carbon fiber has a larger length-diameter ratio, cobalt nanoparticles and manganese oxide nanoparticles can be uniformly distributed in a carbon fiber matrix, and the interface loss of electromagnetic waves when the electromagnetic waves are in contact with the material is increased.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a flow chart of the steps of a carbon/manganese oxide/cobalt nanocomposite fiber material according to an embodiment of the invention;
fig. 2 is a low power scanning electron microscope image of the carbon/manganese oxide/cobalt nanocomposite fibrous material prepared in examples 1-3 of the present invention, wherein (a) is a low power scanning electron microscope image of the carbon/manganese oxide/cobalt nanocomposite fibrous material prepared in example 1, (b) is a low power scanning electron microscope image of the carbon/manganese oxide/cobalt nanocomposite fibrous material prepared in example 2, and (c) is a low power scanning electron microscope image of the carbon/manganese oxide/cobalt nanocomposite fibrous material prepared in example 3.
Fig. 3 is a high power scanning electron microscope image of the carbon/manganese oxide/cobalt nanocomposite fibrous material prepared in examples 1-3 of the present invention, wherein (a) and (b) are high power scanning electron microscope images of the carbon/manganese oxide/cobalt nanocomposite fibrous material prepared in example 1, (c) and (d) are high power scanning electron microscope images of the carbon/manganese oxide/cobalt nanocomposite fibrous material prepared in example 2, and (e) and (f) are high power scanning electron microscope images of the carbon/manganese oxide/cobalt nanocomposite fibrous material prepared in example 1.
FIG. 4 is an energy dispersive X-ray spectroscopy spectrum of a carbon/manganese oxide/cobalt nanocomposite fiber material of example 1 of the present invention;
FIG. 5 is a low power transmission electron micrograph (a), a high power transmission electron micrograph (b), and a selected area electron diffraction micrograph (c) of the carbon/manganese oxide/cobalt nanocomposite fibrous material according to example 1 of the present invention;
FIG. 6 is a graph showing reflection loss when the carbon/manganese oxide/cobalt nanocomposite fiber materials of examples 1 to 3 of the present invention absorb light.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In order to solve the technical problems that impedance matching is poor after a carbon material and a magnetic metal are compounded, electromagnetic waves are inevitably reflected on the surface of the material, and effective absorption of the electromagnetic waves is not facilitated, the invention provides a carbon/manganese oxide/cobalt nano composite fiber, which comprises carbon fibers, cobalt nano particles and manganese oxide nano particles, wherein the cobalt nano particles and the manganese oxide nano particles are attached to the surfaces of the carbon fibers.
In some embodiments, the carbon fibers have a diameter of 200-400 nm;
preferably, the particle size of the cobalt nanoparticles is 20-40 nm;
preferably, the manganese oxide nanoparticles have a particle size of 40-60 nm.
In some embodiments, the cobalt nanoparticles and manganese oxide nanoparticles are uniformly distributed on the surface of the carbon fiber.
In a second aspect, the invention provides a preparation method of the carbon/manganese oxide/cobalt nano composite fiber, which comprises the following steps:
dissolving a cobalt source, a manganese source and a carbon source in an organic solvent to form a spinning solution, spinning the spinning solution to prepare a precursor, and drying, pre-oxidizing and thermally treating the precursor to obtain the catalyst.
In some embodiments, the cobalt source is cobalt acetylacetonate, the manganese source is manganese acetylacetonate, and the carbon source is polyvinylpyrrolidone.
Further, the organic solvent is N, N-dimethylformamide.
Polyvinylpyrrolidone (PVP, model K88-96, molecular weight 1300000) was dissolved in N, N-Dimethylformamide (DMF) solution and magnetically stirred to provide viscosity to the system.
Furthermore, the concentration of polyvinylpyrrolidone in the spinning solution is 0.1-0.2 g/ml; the concentration of cobalt acetylacetonate is 1-3 mmol; the concentration of manganese acetylacetonate is 1-3 mmol.
In some embodiments, the inner diameter of the needle subjected to electrospinning is 20-24 Ga.
Further, the parameters during electrostatic spinning are as follows: the positive electrode is 10-13kV, and the negative electrode is-1 kV; the distance of the collecting plate is 22-26 cm; the spinning temperature is 35-40 deg.C, preferably 39 deg.C.
Further, the drying temperature of the non-woven fabric is 45-55 ℃. The drying is to completely volatilize the residual N, N-Dimethylformamide (DMF) solution on the non-woven fabric, and if the residual N, N-Dimethylformamide (DMF) solution is slightly increased, unnecessary energy waste is caused, and if the residual N, N-Dimethylformamide (DMF) solution is excessively increased, carbon, cobalt and manganese in the non-woven fabric react with oxygen in the air.
Furthermore, the pre-oxidation temperature is 170-190 ℃, and the pre-oxidation time is 1.5-2.5 h.
In some embodiments, the heat treatment is performed in a hydrogen atmosphere with a hydrogen concentration of 3-8%, preferably 5% by volume. Hydrogen is an atmosphere that provides a reducing atmosphere to protect carbon, cobalt and manganese from reacting with oxygen in the air.
Further, the heat treatment temperature is 650-750 ℃, and the heat treatment time is 1.5-2.5 h.
In a third aspect, the invention provides an application of the carbon/manganese oxide/cobalt nano composite fiber wave-absorbing material as an electromagnetic wave absorbing material, especially an application as an electromagnetic wave absorbing material of 2-18 GHz.
The implementation process of the invention is illustrated by several specific application examples.
Example 1
Firstly, weighing 1.4g of polyvinylpyrrolidone K88-96, and dissolving the polyvinylpyrrolidone K88-96 in 10mL of N, N-dimethylformamide solution to form a solution with a certain viscosity; dissolving 2mmol of cobalt acetylacetonate and 2mmol of manganese acetylacetonate in the system, and magnetically stirring to form a spinning solution; after the mixture is uniformly stirred, putting the spinning solution into an electrostatic spinning machine, setting the temperature in the machine to be 39 ℃, the anode to be 12kV, the cathode to be-1 kV, the distance between collecting plates to be 25cm and the size of a needle head to be 22Ga., and carrying out electrostatic spinning to obtain non-woven fabrics; taking out the non-woven fabric, and drying the non-woven fabric in a 50 ℃ oven for 3 hours; placing the mixture in an oven at 180 ℃ for pre-oxidation for 2 h; and finally, placing the pre-oxidized non-woven fabric in a tubular furnace at 700 ℃ in an environment containing 5% of hydrogen for heat treatment to finally obtain the carbon/manganese oxide/cobalt composite nanofiber. The surface of the obtained fiber is rough.
Fig. 2(a) is a low power scanning electron micrograph of the carbon/manganese oxide/cobalt composite nanofiber material of example 1, fig. 3(a) and (b) are high power scanning electron micrographs of the carbon/manganese oxide/cobalt composite nanofiber material of example 1, fig. 4 is an energy dispersive X-ray spectrum of the carbon/manganese oxide/cobalt composite nanofiber material of example 1, and fig. 5 is a low power transmission electron micrograph (a), a high power transmission electron micrograph (b), and a selected area electron diffraction pattern (c) of the carbon/manganese oxide/cobalt composite nanofiber material of example 1; FIG. 6 is a graph of the reflection loss of the carbon/manganese oxide/cobalt nanocomposite fiber material of example 1, with a maximum reflection loss of-71.7 dB at 14.1GHz and 2.3 mm.
Example 2
Firstly, weighing 1.4g of polyvinylpyrrolidone K88-96, and dissolving the polyvinylpyrrolidone K88-96 in 10mL of N, N-dimethylformamide solution to form a solution with a certain viscosity; dissolving 6mmol of cobalt acetylacetonate and 2mmol of manganese acetylacetonate in the system, and magnetically stirring to form a spinning solution; after the mixture is uniformly stirred, putting the spinning solution into an electrostatic spinning machine, setting the temperature in the machine to be 39 ℃, the anode to be 12kV, the cathode to be-1 kV and the distance between collecting plates to be 25cm, and carrying out electrostatic spinning to obtain non-woven fabrics; taking out the non-woven fabric, and drying the non-woven fabric in a 50 ℃ oven for 3 hours; placing the mixture in an oven at 180 ℃ for pre-oxidation for 2 h; and finally, placing the pre-oxidized non-woven fabric in a tubular furnace at 700 ℃ in an environment containing 5% of hydrogen for heat treatment to finally obtain the carbon/manganese oxide/cobalt composite nanofiber. The obtained fiber has smooth surface.
Wherein fig. 2(b) is a low-power scanning electron microscope image of the carbon/manganese oxide/cobalt composite nanofiber material of example 2, and fig. 3(c) and (d) are high-power scanning electron microscope images of the carbon/manganese oxide/cobalt composite nanofiber material of example 2; FIG. 6 is a graph of the reflection loss of the carbon/manganese oxide/cobalt nanocomposite fiber material of example 2, wherein the maximum reflection loss of example 2 is-19.3 dB.
Example 3
Firstly, weighing 1.4g of polyvinylpyrrolidone K88-96, and dissolving the polyvinylpyrrolidone K88-96 in 10mL of N, N-dimethylformamide solution to form a solution with a certain viscosity; dissolving 2mmol of cobalt acetylacetonate and 6mmol of manganese acetylacetonate in the system, and magnetically stirring to form a spinning solution; after the mixture is uniformly stirred, putting the spinning solution into an electrostatic spinning machine, setting the temperature in the machine to be 39 ℃, the anode to be 12kV, the cathode to be-1 kV and the distance between collecting plates to be 25cm, and carrying out electrostatic spinning to obtain non-woven fabrics; taking out the non-woven fabric, and drying the non-woven fabric in a 50 ℃ oven for 3 hours; placing the mixture in an oven at 180 ℃ for pre-oxidation for 2 h; and finally, placing the pre-oxidized non-woven fabric in a tubular furnace at 700 ℃ in an environment containing 5% of hydrogen for heat treatment to finally obtain the carbon/manganese oxide/cobalt composite nanofiber. The resulting fibers were rough in surface with particles of cobalt and manganese oxide present.
Wherein fig. 2(c) is a low-power scanning electron microscope image of the carbon/manganese oxide/cobalt composite nanofiber material of example 3, and fig. 3(e) and (f) are high-power scanning electron microscope images of the carbon/manganese oxide/cobalt composite nanofiber material of example 3; FIG. 6 is a graph of the reflection loss of the carbon/manganese oxide/cobalt nanocomposite fiber material of example 3 of the present invention, the maximum reflection loss of which is-21.4 dB.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A carbon/manganese oxide/cobalt nano composite fiber is characterized in that: comprises carbon fiber, cobalt nanoparticles and manganese oxide nanoparticles attached to the surface of the carbon fiber.
2. The carbon/manganese oxide/cobalt nanocomposite fiber according to claim 1, wherein: the diameter of the carbon fiber is 200-400 nm;
preferably, the particle size of the cobalt nanoparticles is 20-40 nm;
preferably, the manganese oxide nanoparticles have a particle size of 40-60 nm.
3. The carbon/manganese oxide/cobalt nanocomposite fiber according to claim 1, wherein: the cobalt nanoparticles and the manganese oxide nanoparticles are uniformly distributed on the surface of the carbon fiber.
4. A preparation method of carbon/manganese oxide/cobalt nano composite fiber is characterized by comprising the following steps: the method comprises the following steps:
dissolving a cobalt source, a manganese source and a carbon source in an organic solvent to form a spinning solution, spinning the spinning solution to prepare a precursor, and drying, pre-oxidizing and thermally treating the precursor to obtain the catalyst.
5. The method of preparing carbon/manganese oxide/cobalt nanocomposite fibers according to claim 4, wherein: the cobalt source is cobalt acetylacetonate, the manganese source is manganese acetylacetonate, and the carbon source is polyvinylpyrrolidone;
further, the organic solvent is N, N-dimethylformamide;
furthermore, the concentration of polyvinylpyrrolidone in the spinning solution is 0.1-0.2 g/ml; the concentration of cobalt acetylacetonate is 1-3 mmol; the concentration of manganese acetylacetonate is 1-3 mmol.
6. The method of preparing carbon/manganese oxide/cobalt nanocomposite fibers according to claim 4, wherein: the inner diameter of the needle for electrospinning was 20 to 24 Ga.
7. The method of preparing carbon/manganese oxide/cobalt nanocomposite fibers according to claim 4, wherein: the parameters during electrostatic spinning are as follows: the positive electrode is 10-13kV, and the negative electrode is-1 kV; the distance of the collecting plate is 22-26 cm; the spinning temperature is 35-40 deg.C, preferably 39 deg.C.
8. The method of preparing carbon/manganese oxide/cobalt nanocomposite fibers according to claim 4, wherein: the drying temperature of the non-woven fabric is 45-55 ℃;
furthermore, the pre-oxidation temperature is 170-190 ℃, and the pre-oxidation time is 1.5-2.5 h.
9. The method of preparing carbon/manganese oxide/cobalt nanocomposite fibers according to claim 4, wherein: the heat treatment is carried out in a hydrogen atmosphere, the hydrogen concentration is 3-8%, preferably 5%, and the volume percentage is percent;
further, the heat treatment temperature is 650-750 ℃, and the heat treatment time is 1.5-2.5 h.
10. The carbon/manganese oxide/cobalt nano composite fiber wave-absorbing material of any one of claims 1 to 4, which is applied as an electromagnetic wave absorbing material, in particular as an electromagnetic wave absorbing material of 2 to 18 GHz.
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| CN111014712A (en) * | 2019-12-18 | 2020-04-17 | 山东大学 | Co/MnO @ C composite electromagnetic wave absorbing material and preparation method and application thereof |
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| JP2007246317A (en) * | 2006-03-14 | 2007-09-27 | National Institute For Materials Science | Nanocarbon material composite and its manufacturing method |
| CN103422193A (en) * | 2013-08-05 | 2013-12-04 | 江苏科技大学 | Co/C composite nanofiber microwave absorbent, and preparation method and application thereof |
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