CN110723723B - Two-dimensional carbon material loaded Fe 3 N-nanoparticle light wave-absorbing material and preparation method and application thereof - Google Patents

Two-dimensional carbon material loaded Fe 3 N-nanoparticle light wave-absorbing material and preparation method and application thereof Download PDF

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CN110723723B
CN110723723B CN201911199470.4A CN201911199470A CN110723723B CN 110723723 B CN110723723 B CN 110723723B CN 201911199470 A CN201911199470 A CN 201911199470A CN 110723723 B CN110723723 B CN 110723723B
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dimensional carbon
absorbing material
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CN110723723A (en
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吴广磊
周新峰
贾梓睿
冯爱玲
赵修松
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Qingdao University
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    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
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    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C01B21/0615Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
    • C01B21/0622Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with iron, cobalt or nickel
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Abstract

The invention belongs to the technical field of electromagnetic wave-absorbing materials, and particularly relates to a two-dimensional carbon material loaded Fe 3 N nano particle light wave-absorbing material, and a preparation method and application thereof. Adding fish skin into deionized water dissolved Fe (NO) 3 ) 3 ·6H 2 Fully soaking in O, then drying and high-temperature treating to obtain the two-dimensional carbon material loaded Fe 3 N nano-particle light electromagnetic wave-absorbing material. The preparation method has the advantages of wide raw materials, adjustable load capacity, low cost, simple process and the like, and the prepared material has excellent electromagnetic attenuation capability and wider effective absorption bandwidth.

Description

Two-dimensional carbon material loaded Fe 3 N-nanoparticle light wave-absorbing material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of electromagnetic wave-absorbing materials, and particularly relates to a two-dimensional carbon material loaded Fe 3 N nano particle light wave-absorbing material, and a preparation method and application thereof.
Background
With the rapid development of science and technology in the current society, various kinds of electrons are widely used in various fields. Particularly, the development of 5G communication makes the electromagnetic pollution problem more serious, seriously influences the communication system and endangers the health of human bodies, and the solution of the electromagnetic pollution problem is a topic of wide social concern. Therefore, the preparation of the wave-absorbing material with the advantages of high absorption energy efficiency, effective absorption of wide bandwidth, thin matching thickness, environmental friendliness and the like is a key for solving the electromagnetic pollution problem. Generally, electromagnetic wave absorbing materials can be classified into two types according to loss mechanisms: dielectric loss materials (e.g., graphene, carbon nanotubes, etc.) and magnetically loss materials (e.g., fe 3 O 4 、Co 3 O 4 Co, fe, etc.). However, they have respective disadvantages, for example, graphene has a limit to its application to a great extent due to its complicated preparation process, fe 3 O 4 The defects of large density, thick matching thickness, poor performance and the like exist, and the electromagnetic wave-absorbing material is often not used alone. Combining the two into a complexThe composite material is an effective method. However, the disadvantages that the process flow is complex and the reagents used in the experimental process are harmful to human bodies and the environment are still a great difficulty in restricting the application of the reagents.
Disclosure of Invention
The invention aims to provide a two-dimensional carbon material loaded Fe 3 N nano-particle light electromagnetic absorption material, and a preparation method and application thereof.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
two-dimensional carbon material loaded Fe 3 Preparation method of N nanoparticle light wave-absorbing material comprises adding fish skin into deionized water dissolved Fe (NO) 3 ) 3 ·6H 2 Fully soaking in O, then drying and high-temperature treating to obtain the two-dimensional carbon material loaded Fe 3 N nano-particle light electromagnetic wave-absorbing material.
The method comprises the following steps: dissolving ferric nitrate hexahydrate in deionized water, and fully stirring and dissolving; adding fish skin, and soaking in dissolved Fe (NO) 3 ) 3 ·6H 2 O in deionized water; then placing the system in a baking oven for baking, and fully grinding the dried fish skin into powder; and then carrying out high-temperature treatment in a tube furnace, and taking out, washing and drying to obtain the wave-absorbing material.
The Fe (NO) 3 ) 3 ·6H 2 O is dissolved in deionized water, fe (NO 3 ) 3 ·6H 2 The final concentration of O is 0.025-0.1mol/L; the fish skin mass (g) and Fe (NO) 3 ) 3 ·6H 2 The molar ratio of O (mmol) is 1-2:0.1-1.5.
The system is put into an oven for drying at 60-80 ℃; the high temperature treatment temperature is 650-850 ℃ and the treatment time is 1-3 hours.
The fish skin is carp skin.
Two-dimensional carbon material loaded Fe 3 The light electromagnetic wave-absorbing material of the N nano particles is prepared according to the method; the carbon material is in a two-dimensional carbon sheet shape and is uniform in the materialDispersing Fe with octahedral shape and uniform size 3 N nanoparticles.
Two-dimensional carbon material loaded Fe 3 Application of light electromagnetic wave-absorbing material of N nano-particles, wherein the two-dimensional carbon material is loaded with Fe 3 The light electromagnetic wave absorbing material of the N nano particles is applied to the application as a high-efficiency light absorbent.
Two-dimensional carbon material loaded Fe 3 Application of light electromagnetic wave-absorbing material of N nano-particles, wherein the two-dimensional carbon material is loaded with Fe 3 The application of the light electromagnetic wave absorbing material of the N nano particles in treating electromagnetic pollution in daily life.
The invention has the advantages that:
compared with the prior report, the invention uses Fe 3 N is applied to the field of wave-absorbing materials; the two-dimensional carbon material of the invention loads Fe 3 The N nano particle composite material and the two-dimensional carbon nano sheet have excellent conductivity and provide conductive loss for attenuating electromagnetic waves; fe (Fe) 3 The rich interface of N and two-dimensional carbon material provides interfacial polarization loss to attenuate electromagnetic waves. By adjusting Fe 3 The load of N adjusts the dielectric constant of the composite material and then adjusts the impedance matching of the composite material, so that electromagnetic waves can enter the wave absorber more and be consumed. In addition, the preparation method has the advantages of wide raw materials, simple preparation process, low cost, no pollution and the like, is environment-friendly, has no toxic byproducts, provides health assurance for researchers, and further has good electromagnetic attenuation capability.
Drawings
FIG. 1 is a two-dimensional carbon material-supported Fe prepared in examples 1 and 2 of the present invention 3 An X-ray diffraction pattern of the N-nanoparticle light electromagnetic wave-absorbing material;
FIG. 2 is a two-dimensional carbon material-supported Fe prepared in example 1 of the present invention 3 Scanning electron microscope pictures of N nano particle light electromagnetic wave-absorbing materials;
FIG. 3 is a two-dimensional carbon material-supported Fe prepared in example 2 of the present invention 3 Scanning electron microscope pictures of N nano particle light electromagnetic wave-absorbing materials;
FIG. 4 is the presentFe-loaded two-dimensional carbon material prepared in invention example 1 3 Reflection loss spectrogram of the N nano particle light electromagnetic wave-absorbing material;
FIG. 5 is a two-dimensional carbon material-supported Fe prepared in example 2 of the present invention 3 Reflection loss spectrogram of the N nano particle light electromagnetic wave-absorbing material;
FIG. 6 is a two-dimensional carbon material-supported Fe prepared in examples 1 and 2 of the present invention 3 Dielectric loss diagram of N nanoparticle light electromagnetic wave absorbing material.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings, in order to make the objects and technical solutions of the present invention more apparent.
The invention adds Fe (NO) 3 ) 3 ·6H 2 O is dissolved in distilled water, added with fish skin, fully soaked and then placed in an oven. And (5) after the material is completely dried, carrying out high-temperature treatment in a tube furnace, and taking out, washing and drying after the material is naturally cooled to obtain the wave-absorbing material. The preparation method provided by the invention has the advantages of wide selection of the carp skin as the carbon source, simple preparation process, low cost, no pollution and the like, and the composite material prepared by the method has good electromagnetic attenuation capability.
Example 1
Two-dimensional carbon material loaded Fe 3 The preparation method of the N nanoparticle light electromagnetic absorption material comprises the following steps:
step 1, 0.5mmol Fe (NO) was weighed 3 ) 3 ·6H 2 Placing O in 20ml of distilled water, and fully dissolving under magnetic stirring;
and 2, placing 2g of fish skin in the solution obtained in the step 1, fully soaking the fish skin by ultrasonic treatment, and then placing the fish skin in an 80-DEG C oven until the water is completely evaporated.
And 3, fully grinding the dried fish skin to powder after the distilled water in the step 2 is evaporated, and then taking out the powder and placing the powder into a tube furnace for treatment for 1h at 750 ℃ under the atmosphere of nitrogen.
And 4, after the heat treatment in the step 3 is completed, taking out, washing with deionized water, and drying at 60 ℃ to obtain a required product (see fig. 1, 2, 4 and 6).
Examples2:
Two-dimensional carbon material loaded Fe 3 The preparation method of the N nanoparticle light electromagnetic absorption material comprises the following steps:
step 1, 1.0mmol Fe (NO) was weighed out 3 ) 3 ·6H 2 Placing O in 20ml of distilled water, and fully dissolving under magnetic stirring;
and 2, placing 2g of fish skin in the solution obtained in the step 1, fully soaking the fish skin by ultrasonic treatment, and then placing the fish skin in an 80-DEG C oven until the water is completely evaporated.
And 3, fully grinding the dried fish skin to powder after the distilled water in the step 2 is evaporated, and then placing the powder into a tube furnace for treatment at 750 ℃ for 1h, wherein the atmosphere is nitrogen.
And 4, after the heat treatment in the step 3 is completed, taking out, washing with deionized water, and drying at 60 ℃ to obtain a required product (see fig. 1, 3, 5 and 6).
FIG. 1 shows a two-dimensional carbon material-supported Fe of example 1 and example 2 3 XRD patterns of the N nano particle light electromagnetic absorption material correspond to diffraction peaks at 43.5 DEG and 41.1 DEG and are Fe 3 N has (111) and (002) crystal planes (PDF- # 83-0877). And as the amount of the ferric salt increases, the intensity of the diffraction peak increases, proving Fe 3 The crystallinity of N is also increasing.
FIG. 2 and FIG. 3 are each a scanning electron microscope photograph of embodiment 1 and embodiment 2, respectively, from which it can be seen that Fe is produced with increasing amount of iron salt 3 The number of N particles is also increasing. Most of Fe 3 The N particles have an octahedral structure and have a particle size of about 200 nm.
Application example:
the samples obtained in examples 1 and 2 were uniformly mixed with paraffin wax in a mass ratio of 1:4, pressed into circular rings with an inner diameter of 3.04mm, an outer diameter of 7.00mm and a thickness of about 2.00mm by a mold, respectively measured for electromagnetic parameters by a vector grid analyzer, and then subjected to simulation calculation to obtain reflection loss spectrograms of the materials (see fig. 4, 5 and 6).
FIG. 4 and FIG. 5 are reflected losses for example 1 and example 2, respectivelyThe sample loading calculated by the formula was a reflection loss spectrum of 20%. As can be seen from the figure, the sample obtained in example 1 has a reflection loss extremum of-57.5 dB at 2.9 mm; however, the reflection loss of example 2 at a thickness of 0.1 to 5mm is less than-10 dB, and the practical application is not satisfied. It is apparent that the electromagnetic wave-absorbing property of example 1 is far greater than that of example 2, and the difference between the two is mainly due to Fe 3 Different N loading amounts, fe 3 The interface between the N nano particles and the carbon nano sheets is increased, so that the transmission of electrons is influenced, and the dielectric constant of the material is influenced.
Fig. 6 is a comparison of the dielectric loss capacities of embodiment 1 and embodiment 2, and it is apparent that the dielectric loss of embodiment 2 is much smaller than that of embodiment 1, and it is shown that the dielectric loss capacity of embodiment 1 for electromagnetic waves is much greater than that of embodiment 2, and the obtained results are consistent with the electromagnetic wave absorption performance of the embodiment corresponding to fig. 4 and 5.
It is apparent that the above examples are only illustrative of the present invention and are not limiting of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious changes and modifications which come within the spirit of the invention are desired to be protected.

Claims (5)

1. Two-dimensional carbon material loaded Fe 3 The preparation process of light N-nanometer particle wave absorbing material features that fish skin is added into deionized water dissolved Fe (NO) 3 ) 3 ·6H 2 Fully soaking in O, then drying and high-temperature treating to obtain the two-dimensional carbon material loaded Fe 3 N nano-particle light electromagnetic wave-absorbing material;
the Fe (NO) 3 ) 3 ·6H 2 O is dissolved in deionized water, fe (NO 3 ) 3 ·6H 2 The final concentration of O is 0.025-0.1mol/L; the fish skin mass (g) and Fe (NO) 3 ) 3 ·6H 2 O mole number (mmol)The ratio is 1-2:0.1-1.5;
dissolving ferric nitrate hexahydrate in deionized water, and fully stirring and dissolving; adding fish skin, and soaking in dissolved Fe (NO) 3 ) 3 ·6H 2 O in deionized water; then placing the system in a baking oven for baking, and fully grinding the dried fish skin into powder; then, carrying out high-temperature treatment in a tube furnace, and taking out, washing and drying to obtain the wave-absorbing material;
the system is put into an oven for drying at 60-80 ℃; the high temperature treatment temperature is 650-850 ℃ and the treatment time is 1-3 hours.
2. The two-dimensional carbon material-supported Fe as defined in claim 1 3 The preparation method of the light electromagnetic wave-absorbing material with the N nano particles is characterized in that the fish skin is carp skin.
3. A two-dimensional carbon material-supported Fe of claim 1 3 The light electromagnetic wave-absorbing material of N nano particles, which is characterized in that the light electromagnetic wave-absorbing material is prepared by the method of claim 1; the carbon material is in a two-dimensional carbon sheet shape, and Fe with octahedral shape and uniform size is uniformly dispersed in the material 3 N nanoparticles.
4. A two-dimensional carbon material-supported Fe of claim 3 3 The application of the light electromagnetic wave-absorbing material of the N nano-particles is characterized in that the two-dimensional carbon material is loaded with Fe 3 The light electromagnetic wave absorbing material of the N nano particles is applied to the application as a high-efficiency light absorbent.
5. A two-dimensional carbon material-supported Fe as claimed in claim 4 3 The application of the light electromagnetic wave-absorbing material of the N nano-particles is characterized in that the two-dimensional carbon material is loaded with Fe 3 The application of the light electromagnetic wave absorbing material of the N nano particles in treating electromagnetic pollution in daily life.
CN201911199470.4A 2019-11-29 2019-11-29 Two-dimensional carbon material loaded Fe 3 N-nanoparticle light wave-absorbing material and preparation method and application thereof Active CN110723723B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110269250A1 (en) * 2010-05-03 2011-11-03 Nanjing University Growth method of fe3n material

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CN107033842B (en) * 2017-05-16 2019-03-01 山东大学 A kind of composite wave-absorbing agent, preparation method and applications
CN110358500B (en) * 2019-07-22 2022-08-02 青岛大学 Preparation method and application of porous carbon-loaded cobaltosic oxide-coated cobalt alloy wave-absorbing material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110269250A1 (en) * 2010-05-03 2011-11-03 Nanjing University Growth method of fe3n material

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