CN114051368A - Loofah fiber electromagnetic wave absorbing material and preparation method thereof - Google Patents

Loofah fiber electromagnetic wave absorbing material and preparation method thereof Download PDF

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Publication number
CN114051368A
CN114051368A CN202110665383.4A CN202110665383A CN114051368A CN 114051368 A CN114051368 A CN 114051368A CN 202110665383 A CN202110665383 A CN 202110665383A CN 114051368 A CN114051368 A CN 114051368A
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China
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electromagnetic wave
wave absorbing
absorbing material
loofah
fibers
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叶伟
张杏
孙启龙
龙啸云
高强
季涛
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Nantong University
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Nantong University
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073Shielding materials
    • H05K9/0081Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/0083Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01QANTENNAS, i.e. RADIO AERIALS
    • H01Q17/00Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
    • H01Q17/004Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems using non-directional dissipative particles, e.g. ferrite powders

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Manufacturing & Machinery (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention belongs to the field of preparation of electromagnetic wave absorbing materials, and particularly discloses a loofah fiber electromagnetic wave absorbing material and a preparation method thereof, wherein natural loofah fibers are used as base materials, the fibers are hollow and are provided with grooves on the surfaces, in-situ hybridization is carried out on the fibers to generate magnetic particles with electromagnetic wave absorbing performance, the magnetic particles are magnetic loss particles of ferroferric oxide, iron cobalt and iron nickel, and effective absorption in a frequency band of 6-17 GHz can be realized. The loofah fibers used in the invention exist in a large amount in nature, and have lower cost and greater environmental protection advantages compared with other chemical fibers, the preparation method can combine the advantages of the magnetic particles and the mesoporous carbon-based material, so that the electromagnetic wave absorbing material has better impedance matching property, better wave absorbing effect, lighter carbon magnetic fiber mass, low density and good physical and chemical stability; and the electromagnetic wave absorption efficiency reaches-28 dB at 15.8GHz by adjusting the loading of the magnetic particles on the fiber and the thickness of the sample.

Description

Loofah fiber electromagnetic wave absorbing material and preparation method thereof
Technical Field
The invention belongs to the field of preparation of electromagnetic wave absorbing materials, and particularly relates to a loofah fiber electromagnetic wave absorbing material and a preparation method thereof.
Background
With the rapid development of electronic and electrical technologies, the range of electromagnetic energy utilization is expanding, and the electromagnetic radiation pollution follows. The problem of electromagnetic pollution has become the 5 th public nuisance following waste water, waste gas, solid waste and noise, and reports have shown that electromagnetic pollution in this century will replace noise pollution and become the first leading physical pollution. At present, the use of electromagnetic wave absorbing materials to reduce or eliminate electromagnetic wave pollution is an effective method.
Compared with the conventional ferrite, carbonyl iron and magnetic electromagnetic wave absorbing material, the carbon-based electromagnetic wave absorbing material has the advantages of light weight, adjustable frequency range and good compatibility with the organic/inorganic phase interface of the matrix, but has the problem that the carbon-based material has too high electrical conductivity to affect the absorption of the electromagnetic wave, such as the article (1) PRASAD J, SINGH a K, tomam, et al. Strong electromagnetic wave absorption and microwave shielding in the Ni-Cu @ MoS 2/rGO composite [ J ]. Journal of Materials Science: Materials in Electronics, 2019, 30(20): 66-77., [2] HE P, HOU Z L, ZHANG K L, et al. light dielectric oxide waveguide fiber and fiber composite [ J ], 2017, 52(13) < 1-10 >, [3] WAN Y, JIAN X, LI C, et al. Microwave absorption properties of FeCo-coated carbon fibers with varying morphology [ J ]. Journal of Magnetic & Magnetic Materials, 2016, 399(FEB.): 252-9.).
Chinese invention patent CN202011254197.3 discloses a carbon-based porous composite wave absorbing agent based on natural loofah and a preparation method thereof, wherein natural loofah is firstly soaked in an aqueous solution of ferric nitrate, ferric chloride or ferric sulfate, then a carbon-based wave absorbing material with a multi-stage porous structure is obtained by a one-step carbonization method, the diameter of the fiber of the calcined loofah is between 200 and 300 mu m, nanoscale iron or oxide particles thereof are uniformly distributed on the surface and inside of the fiber, and the material has high dielectric loss and good impedance matching property, thereby having good wave absorbing performance. However, according to the technical scheme, on one hand, degumming treatment is not carried out, so that the later-stage magnetic particle load strength is not high, and on the other hand, electromagnetic wave loss performance is insufficient due to the fact that ferroferric oxide is used as a single magnetic loss material.
Disclosure of Invention
Aiming at the defects of the prior art, the natural towel gourd fiber is used as a base material, the magnetic particles with electromagnetic wave absorption performance are generated by in-situ hybridization on the fiber, the electromagnetic wave absorption performance of the material can be obviously improved, the natural towel gourd fiber can be used as an electromagnetic wave absorbent to be widely compounded with ceramics, resin and the like to prepare an effective electromagnetic wave protection composite material, and the natural towel gourd fiber has a good application prospect.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a loofah fiber electromagnetic wave absorption material is characterized in that natural loofah fibers are used as base materials, the fibers are hollow and provided with grooves on the surfaces, in-situ hybridization is carried out on the fibers to generate magnetic particles with electromagnetic wave absorption performance, and the magnetic particles are magnetic loss particles such as ferroferric oxide, iron cobalt and iron nickel.
Furthermore, the material can realize effective absorption in the frequency band of 6-17 GHz.
The preparation method of the loofah fiber electromagnetic wave absorbing material comprises the following specific steps:
(1) treating natural towel gourd fibers in a sodium hydroxide solution, keeping a certain temperature, and then cleaning and drying to prepare S1;
(2) treating S1 in hydrogen peroxide, keeping a certain temperature, and then cleaning and drying to prepare S2;
(3) preparing a metal salt solution S3, wherein solutes of the metal salt solution are ferric chloride, nickel carbonate, cobalt nitrate and glucose;
(4) soaking S2 in S3 solution, and drying to obtain S4;
(5) carbonizing S4 to obtain S5 with magnetic particles.
Further, in the step (1), the concentration of the sodium hydroxide solution is 5-7 mol/L; the treatment time is 5 hours; the temperature was maintained at 80 ℃.
Further, in the step (2), the concentration of the hydrogen peroxide is 5-10%; the treatment time was 10 hours.
Further, in the step (2), the temperature is kept at 50-60 ℃.
Further, in the step (3), the concentration of ferric chloride is 0.5-2 mol/L, the concentration of nickel carbonate is 0.1-2 mol/L, the concentration of cobalt nitrate is 0.1-2 mol/L, and the concentration of glucose is 0.1 mol/L.
Further, in the step (4), the soaking time is 5 hours, and the drying temperature is 100 ℃.
Further, in the step (5), the carbonization temperature is 800-900 ℃, and the carbonization time is 3 hours.
Further, in the step (5), nitrogen is introduced for protection in the carbonization process.
Has the advantages that:
1) the loofah fiber carbon-based electromagnetic wave absorbing material prepared by the invention uses loofah fibers which exist in large quantities in nature, and has lower cost and greater environmental protection advantage compared with other chemical fibers; 2) the natural porous hollow towel gourd fiber is used as a carrier, and the carbon/magnetic fiber prepared by the in-situ hybridization process is lighter in weight, has low density and good physical and chemical stability compared with ferrite materials such as ferroferric oxide and carbonyl iron, and can be combined with the advantages of magnetic particles and a mesoporous carbon-based material, so that the electromagnetic wave absorbing material has better impedance matching characteristic and better effect; 3) according to the invention, degumming treatment is firstly carried out, so that particles can be more directly contacted with the loofah carbon fibers after carbonization to form an effective interface effect, and different magnetic loss particles are formed by taking iron salt, cobalt salt and nickel salt as main magnetic loss raw materials, so that the interface is rich and a synergistic effect is formed, the loss of electromagnetic waves of the material is enhanced, and the effective loss bandwidth is wider; 4) samples with different thicknesses are prepared by adjusting the loading amount of magnetic particles on the fibers and mixing the fibers as a wave absorbing agent with resin and the like, so that the electromagnetic waves can be effectively absorbed in a 6-17 GHz band, and the electromagnetic wave absorption efficiency at 15.8GHz reaches-28 dB.
Drawings
FIG. 1 is a scanning electron microscope image of the electromagnetic wave absorbing material of the silk melon fiber in example 1;
FIG. 2 is a graph showing the electromagnetic wave absorption curve of the electromagnetic wave absorption material of the silk melon fiber in example 1;
FIG. 3 is a scanning electron micrograph of the electromagnetic wave absorbing material of the cucurbita pepo fibers in example 2;
FIG. 4 is a graph showing the electromagnetic wave absorption curve of the electromagnetic wave absorption material of the silk melon fiber in example 2;
FIG. 5 is a scanning electron micrograph of the electromagnetic wave absorbing material of the cucurbita pepo fibers in example 3;
fig. 6 is an electromagnetic wave absorption curve diagram of the electromagnetic wave absorption material of the cucurbita pepo fibers in example 3.
Detailed Description
The present invention will be described in further detail with reference to examples. The reagents or instruments used are not indicated by manufacturers, and are regarded as conventional products which can be purchased in the market.
Example 1
(1) Putting natural towel gourd fibers into 5mol/L sodium hydroxide solution for treatment for 5 hours, keeping the temperature at 80 ℃, and then cleaning and drying to prepare S1;
(2) then treating the mixture in 10 percent hydrogen peroxide for 10 hours, keeping the temperature at 50 ℃, and then cleaning and drying the mixture;
(3) preparing a metal salt solution, wherein each liter of the metal salt solution contains 2mol of ferric chloride, 0.1mol of nickel carbonate, 0.1mol of cobalt nitrate and 0.1mol of glucose;
(4) soaking in metal salt solution for 5 hr, and oven drying at 100 deg.C;
(5) then carbonizing at 900 deg.C for 3 hr, introducing N2And protecting to obtain the carbon/magnetic fiber material with the magnetic particles.
Fig. 1 is a scanning electron microscope picture of the electromagnetic wave absorbing material of loofah fibers prepared in example 1, and fig. 1 shows that magnetic particles are uniformly distributed on the fiber surface.
Fig. 2 shows the wave absorbing performance of the loofah fiber electromagnetic wave absorbing material in example 1, and fig. 2 shows the electromagnetic wave absorbing performance of the test sample when the thickness of the test sample is 1mm, 2mm, 3mm, 4mm, and 5mm, respectively, when the thickness is 3mm, the lowest loss of the electromagnetic wave is-22.5 dB, and the loss of the electromagnetic wave is less than-10 dB within the frequency band range of 6.5 to 9.5 GHz.
Example 2
(1) Putting natural towel gourd fibers into 7mol/L sodium hydroxide solution for treatment for 5 hours, keeping the temperature at 80 ℃, and then cleaning and drying to prepare S1;
(2) treating S1 in 5% hydrogen peroxide for 10 hr, maintaining the temperature at 60 deg.c, washing and stoving to prepare S2;
(3) preparing a metal salt solution S3, wherein each liter of metal salt solution contains 2mol of ferric chloride, 2mol of cobalt nitrate and 0.1mol of glucose;
(4) soaking S2 in S3 solution for 5 hours, and drying at 100 ℃ to obtain S4;
(5) carbonizing S4 at 800 deg.C for 3 hr, introducing N2Protection, S5 with magnetic particles was obtained.
Fig. 3 is a scanning electron microscope picture of the electromagnetic wave absorbing material of loofah fibers prepared in example 2, and fig. 3 shows that magnetic particles are uniformly distributed on the fiber surface.
Fig. 4 shows the wave absorbing performance of the electromagnetic wave absorbing material of loofah fiber in example 2, and fig. 4 shows the electromagnetic wave absorbing performance of the test sample when the thickness of the test sample is 1mm, 2mm, 3mm, 4mm and 5mm, when the thickness is 5mm, the lowest loss of the electromagnetic wave is-31.5 dB, and an effective waveband that the loss of the electromagnetic wave is less than-10 dB exists in the test sample with the thickness of 2-5 mm.
Example 3
(1) Putting natural towel gourd fibers into 5mol/L sodium hydroxide solution for treatment for 5 hours, keeping the temperature at 80 ℃, and then cleaning and drying to prepare S1;
(2) treating S1 in 10% hydrogen peroxide for 10 hr, maintaining the temperature at 50 deg.c, washing and stoving to prepare S2;
(3) preparing a metal salt solution S3, wherein each liter of the metal salt solution contains 0.5mol of ferric chloride, 1mol of nickel carbonate, 2mol of cobalt nitrate and 0.1mol of glucose;
(4) soaking S2 in S3 solution for 5 hours, and drying at 110 ℃ to obtain S4;
(5) carbonizing S4 at 800 deg.C for 3 hr, introducing N2Protection, S5 with magnetic particles was obtained.
Fig. 5 is a scanning electron microscope picture of the electromagnetic wave absorbing material of loofah fibers prepared in example 3, and fig. 5 shows that magnetic particles are uniformly distributed on the fiber surface.
Fig. 6 shows the wave-absorbing performance of the loofah fiber electromagnetic wave absorbing material of example 3, and fig. 6 shows the electromagnetic wave absorbing performance of the test sample when the thickness of the test sample is 1mm, 2mm, 3mm, 4mm, and 5mm, where the lowest loss of the electromagnetic wave is-21.2 dB when the thickness of the test sample is 4mm, and the loss of the electromagnetic wave is less than-10 dB in the frequency range of 8.8 to 16.6GHz when the thickness of the test sample is 2 mm.
The protection of the present invention is not limited to the above embodiments. Variations and advantages that may occur to those skilled in the art may be incorporated into the invention without departing from the spirit and scope of the inventive concept and the scope of the appended claims is intended to be protected.

Claims (10)

1. A loofah fiber electromagnetic wave absorbing material is characterized in that: the material is prepared by taking natural towel gourd fibers as a base material, wherein the fibers are hollow and provided with grooves on the surfaces, in-situ hybridization is carried out on the fibers to generate magnetic particles with electromagnetic wave absorption performance, and the magnetic particles are magnetic loss particles of ferroferric oxide, iron cobalt and iron nickel.
2. The electromagnetic wave absorbing material of loofah fiber according to claim 1, characterized in that: the material can realize effective absorption in the frequency band of 6-17 GHz.
3. The method for preparing the electromagnetic wave absorbing material of loofah fiber according to any one of claims 1 to 2, comprising the steps of: the method comprises the following specific steps:
(1) treating natural towel gourd fibers in a sodium hydroxide solution, keeping a certain temperature, and then cleaning and drying to prepare S1;
(2) treating S1 in hydrogen peroxide, keeping a certain temperature, and then cleaning and drying to prepare S2;
(3) preparing a metal salt solution S3, wherein solutes of the metal salt solution are ferric chloride, nickel carbonate, cobalt nitrate and glucose;
(4) soaking S2 in S3 solution, and drying to obtain S4;
(5) carbonizing S4 to obtain S5 with magnetic particles.
4. The method for preparing the electromagnetic wave absorbing material of loofah fibers according to claim 3, wherein the method comprises the following steps: in the step (1), the concentration of the sodium hydroxide solution is 5-7 mol/L; the treatment time is 5 hours; the temperature was maintained at 80 ℃.
5. The method for preparing the electromagnetic wave absorbing material of loofah fibers according to claim 3, wherein the method comprises the following steps: in the step (2), the concentration of the hydrogen peroxide is 5-10%; the treatment time was 10 hours.
6. The method for preparing the electromagnetic wave absorbing material of loofah fibers according to claim 3, wherein the method comprises the following steps: in the step (2), the temperature is kept at 50-60 ℃.
7. The method for preparing the electromagnetic wave absorbing material of loofah fibers according to claim 3, wherein the method comprises the following steps: in the step (3), the concentration of the ferric chloride is 0.5-2 mol/L, the concentration of the nickel carbonate is 0.1-2 mol/L, the concentration of the cobalt nitrate is 0.1-2 mol/L, and the concentration of the glucose is 0.1 mol/L.
8. The method for preparing the electromagnetic wave absorbing material of loofah fibers according to claim 3, wherein the method comprises the following steps: in the step (4), the soaking time is 5 hours, and the drying temperature is 100 ℃.
9. The method for preparing the electromagnetic wave absorbing material of loofah fibers according to claim 3, wherein the method comprises the following steps: in the step (5), the carbonization temperature is 800-900 ℃, and the carbonization time is 3 hours.
10. The method for preparing the electromagnetic wave absorbing material of loofah fibers according to claim 3, wherein the method comprises the following steps: and (5) introducing nitrogen for protection in the carbonization process.
CN202110665383.4A 2021-06-16 2021-06-16 Loofah fiber electromagnetic wave absorbing material and preparation method thereof Pending CN114051368A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114687009A (en) * 2022-04-21 2022-07-01 南京理工大学 Method for preparing Cu/C hollow wave-absorbing fiber by using kapok fiber

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Publication number Priority date Publication date Assignee Title
CN114687009A (en) * 2022-04-21 2022-07-01 南京理工大学 Method for preparing Cu/C hollow wave-absorbing fiber by using kapok fiber
CN114687009B (en) * 2022-04-21 2024-01-05 南京理工大学 Method for preparing Cu/C hollow wave-absorbing fiber by using kapok fiber

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