CN114752351A - Multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material and preparation method thereof - Google Patents
Multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material and preparation method thereof Download PDFInfo
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- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 title claims abstract description 84
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- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 3
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- GPKIXZRJUHCCKX-UHFFFAOYSA-N 2-[(5-methyl-2-propan-2-ylphenoxy)methyl]oxirane Chemical compound CC(C)C1=CC=C(C)C=C1OCC1OC1 GPKIXZRJUHCCKX-UHFFFAOYSA-N 0.000 description 1
- 241000931705 Cicada Species 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
-
- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses a multidimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material and a preparation method thereof, wherein the porous carbon sheet matrix is obtained by high-temperature pyrolysis of sheets of paper serving as a precursor, and then a cobaltosic oxide magnetic component with adjustable morphology is loaded on the porous carbon sheet by a method combining hydrothermal and thermal treatment, so as to finally obtain a series of multidimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing materials, the special microstructure endows the composite material with an ideal magnetoelectric common loss mechanism and rich interface polarization effects, and simultaneously further optimizes the impedance matching characteristic and the attenuation capability of a system, wherein the needle-shaped cobaltosic oxide array/biomass-based porous carbon sheet composite material has the characteristics of strong reflection loss and wide absorption band under the condition of relatively thin thickness, the wave-absorbing material is excellent, and in addition, the preparation method disclosed by the invention is simple and safe in process, low in cost, green and environment-friendly, so that the wave-absorbing material has a good application value.
Description
Technical Field
The invention relates to an electromagnetic absorption material in the field of functional materials, in particular to a multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material and a preparation method thereof.
Background
In recent years, the rapid development of wireless electronic communication technology and equipment brings convenience to human beings, and the following problems of electromagnetic wave interference and pollution also seriously affect the operation of surrounding precision equipment and human health. Therefore, a light, broadband, strong absorbing and thin absorbing material is urgently needed to solve the problems. Such materials, which can effectively attenuate electromagnetic waves, can be classified into dielectric loss type wave-absorbing materials and magnetic loss type wave-absorbing materials according to their loss mechanisms. However, the above materials with single component have the disadvantages of poor impedance matching or weak attenuation capability, and thus cannot meet the requirements of "light, thin, strong and wide", so that the construction of the composite wave-absorbing material with both magnetic loss and electrical loss becomes a hot point of research. Research shows that the effective combination of the two can solve the problem of impedance mismatch on one hand, so that more electromagnetic waves can enter the composite material, and on the other hand, under the control of various loss mechanisms and interface effects, the electromagnetic waves can be quickly lost and converted into energy in other forms, so that the wave-absorbing performance of the composite material is improved to a great extent. Unfortunately, most of the preparation processes of the composite materials are relatively complex, high in cost and low in yield, and cannot meet the actual requirements. Meanwhile, how to design the microstructure of the material and adjust and control the component proportion to avoid the phenomena of uneven distribution, agglomeration, excessive proportion and the like of the magnetic particles on the carbon matrix to cause overlarge density and poor performance of the final composite material is also a problem to be solved urgently at present.
Compared with the traditional carbon material, the biomass carbon is widely pursued in the field of electromagnetic absorption as a novel material with low cost, reproducibility and environmental friendliness. Particularly, most biomasses have unique microstructures such as porous structures, layered structures, hollow tubular structures and the like, structural diversity can be reserved through simple high-temperature carbonization, and meanwhile, the carbon surface of the biomasses often contains a large number of oxygen-containing functional groups, so that metal ions are favorably attracted, and the magnetic carbon-based composite material is successfully formed. Researches find that the biomass carbon material containing the porous structure is not only beneficial to multiple reflection of electromagnetic waves and improvement of impedance matching, but also can reduce the overall density of the material. Currently, there are still significant challenges to the development of magnetic biomass-based carbon composites.
Disclosure of Invention
Aiming at the technical current situation, the invention provides a multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material and a preparation method thereof.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material is composed of a multi-dimensional cobaltosic oxide array and a biomass-derived porous carbon sheet, wherein the shape of a multi-dimensional cobaltosic oxide array unit is one of needle shape, sheet shape and sea urchin ball shape, and the biomass source of the porous carbon sheet is millettia paper.
The invention provides a preparation method of a multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material, which comprises the following steps:
Wherein the heating rate of the calcination in the step 1 is 1-10 ℃/min, the calcination temperature is 600-800 ℃, the calcination time is 90-180 min, and the protective atmosphere is one or more selected from argon and nitrogen.
Wherein, in the step 2, the mass ratio of the porous carbon sheet, the cobalt nitrate hexahydrate, the urea, the ammonium fluoride and the deionized water is 1: (0.72-2.18): (0.75-2.25): (0.38-1.13): (100-300); the hydrothermal reaction temperature is 100-130 ℃, and the reaction time is 360-720 min; the calcination temperature is 300-450 ℃, and the calcination time is 120-240 min.
Compared with the prior art, the technical scheme of the invention has the beneficial effects that:
1. the invention adopts high-temperature pyrolysis and hydrothermal reaction to prepare the multidimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material, and the method has the advantages of simple and safe operation, low cost and environmental protection.
2. The invention can realize the transformation of the cobaltosic oxide array appearance from sea urchin sphere shape to sheet shape and needle shape by simply changing the hydrothermal reaction condition, thereby realizing the effective regulation and control of electromagnetic parameters and wave absorption performance.
3. The needle-shaped cobaltosic oxide/biomass-based porous carbon sheet composite material prepared by the invention has excellent electromagnetic absorption performance. Under the magnetoelectric common loss mechanism, rich interface effect and optimized impedance matching effect, the minimum reflection loss value of the absorbent reaches-60.5 dB, and the effective absorption bandwidth reaches 6.8 GHz.
Drawings
FIG. 1 XRD patterns of examples 1-3 and comparative examples;
FIG. 2 SEM (top) and TEM (bottom) images of examples 1-3 and comparative examples;
FIG. 3 shows the wave-absorbing properties of examples 1 to 3 and comparative examples.
Detailed Description
The invention will be described in further detail below with reference to the embodiments of the drawing, which are intended to facilitate the understanding of the invention and are not intended to limit the invention in any way.
The invention provides the following specific embodiments, discloses the performance of various combination examples, and analyzes the effect of each experimental parameter in the system. Therefore, this patent specification should be considered to disclose all possible combinations of the described technical solutions.
Example 1:
in the embodiment, the prepared product is a sea urchin spherical cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material.
The preparation method of the sea urchin spherical cobaltosic oxide array/biomass-based porous carbon sheet composite material comprises the following steps:
The product obtained above was tested as follows:
(A) respectively adopts an irradiation source of Cu-Ka ()λ1.54 a) (abbreviated as XRD, the same applies hereinafter) to determine the crystal structure of the sample.
(B) And observing the microscopic morphology of the sample by adopting a scanning electron microscope (SEM for short) and a transmission electron microscope (TEM for short).
(C) Electromagnetic parameters (complex permittivity and complex permeability) of the material were determined by a ceyear 3672B-S vector network analyzer in the frequency range of 2-18 GHz. Preparation of a test sample: the product was uniformly mixed with paraffin wax to a total weight of 35% and then pressed into a ring (outer diameter: 7.0 mm, inner diameter: 3.04 mm).
Example 2:
in the embodiment, the prepared product is a flaky cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material.
The preparation method of the flaky cobaltosic oxide array/biomass-based porous carbon sheet composite material comprises the following steps:
Example 3:
in the embodiment, the prepared product is a needle-shaped cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material.
The preparation method of the flaky cobaltosic oxide array/biomass-based porous carbon sheet composite material comprises the following steps:
Comparative example:
this example is a comparative example of the above examples 1, 2, 3.
In this example, the product produced was a biomass-based porous carbon sheet material.
The preparation method of the biomass-based porous carbon sheet material comprises the following steps:
ultrasonically cleaning the oroxylum indicum by using deionized water and absolute ethyl alcohol for 3 times respectively, and then drying the oroxylum indicum in an oven at 60 ℃ for 12 hours; and (3) heating the dried millets to 700 ℃ at the speed of 5 ℃/min in the argon atmosphere, calcining for 120 min, and cooling to room temperature along with the furnace to obtain the biomass-based porous carbon sheet material.
The product prepared by the method is detected, and the contents of the XRD and SEM/TEM detection methods are completely the same as those of the example 1.
The phase change of the materials prepared in examples 1 to 3 and comparative example is shown in fig. 1, the micro-morphology of the materials prepared in examples 1 to 3 and comparative example is shown in fig. 2, and the wave absorption properties of the materials prepared in examples 1 to 3 and comparative example are shown in table 1 below, and the results are shown in fig. 3.
Table 1: reflection loss and wave absorption performance tables in examples 1-3 and comparative examples
The symbols in table 1 have the following meanings:
RL-reflection losses;RL min minimum reflection losses.
Phase analysis: as shown in FIG. 1, the samples obtained in examples 1 to 3 each consist of two phases, tricobalt tetraoxide and graphitized carbon, whereas the comparative examples show only typical diffraction peaks of graphite.
And (3) analyzing change of the micro morphology: as shown in fig. 2, the cobaltosic oxide array units in examples 1-3 respectively exhibit sea urchin sphere, flake and needle shapes and uniformly cover the surface of the porous carbon sheet matrix with the changes of the hydrothermal reaction time and the ammonium fluoride concentration, which indicates that the change of the hydrothermal conditions in the present invention can realize the control of the product micro-morphology. Wherein the average diameter of sea urchin spherical cobaltosic oxide is 8-12 mu m, the thickness of the flaky cobaltosic oxide is 80-100 nm, and the length of the needle-shaped cobaltosic oxide is 4-6 mu m; the porous carbon sheet prepared in the comparative example is microscopically flat like a cicada wing, the surface of the porous carbon sheet is provided with folds and holes, and the aperture range is 20-60 mu m.
And (3) wave absorption performance analysis: it can be seen from table 1 and fig. 3 that when the load is 35%, i.e. the mass of the wave-absorbing composite material of the present invention is 35%, and the mass of the binder is 65%, wherein one of the binder epoxy or paraffin is obviously improved along with the transformation of the cobaltosic oxide on the surface from sea urchin spherical to sheet and needle, the wave-absorbing performance of the sample, especially the range of the effective absorption bandwidth. In the measured frequency range, the RLmin value of the sample at the position of 3.5 mm prepared in the embodiment 1 is only-12.5 dB, and the effective absorption bandwidth is only 1 GHz, which indicates that the sample does not have good wave-absorbing performance; at a coating thickness of 2.5 mm, the effective absorption bandwidth of the sample prepared in example 2 reached 5.7 GHz, but the value of the reflection RLmin at 4mm was only-17.9 dB; in contrast, the sample prepared in example 3 shows excellent reflection loss (-60.5 dB) under the condition that the matching thickness is 2.44 mm, and the wave-absorbing bandwidth is increased to 6.8 GHz. Therefore, the product obtained in the example 3 shows excellent wave-absorbing performance in a C-Ku frequency band (4-18Ghz), when the mass ratio of the ammonium fluoride to the porous carbon exceeds 1.13, the obtained cobaltosic oxide is unevenly distributed in the porous carbon and is agglomerated, so that the wave-absorbing performance is deteriorated, and meanwhile, the components and the structure designed by the invention can realize controllability of electromagnetic parameters and wave-absorbing characteristics, so that the product has great application potential, and the reflection loss (-53.5 dB) and the wave-absorbing bandwidth of the sample prepared in the comparative example are 4.4GHz under the condition that the matching thickness is 2 mm.
In conclusion, the multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material can be prepared through simple heat treatment and hydrothermal reaction, particularly, the process parameters can effectively adjust the microstructure of the system, and the magnetoelectric loss synergistic effect and the optimized impedance matching can be realized, so that the final wave-absorbing performance is improved. Among them, the excellent electromagnetic wave absorption characteristics exhibited by the acicular cobaltosic oxide array/biomass-based porous carbon sheet composite material can be attributed to its specific microstructure and appropriate component proportions. Therefore, the composite material is an ideal wave-absorbing material and can be applied to practical application.
The technical solution of the present invention is described in detail in the foregoing embodiments, and it should be understood that the above-mentioned examples are only specific embodiments of the present invention and are not intended to limit the present invention. Any modification, addition or equivalent substitution made within the scope of the principle of the present invention shall be included in the protection scope of the present invention.
Claims (4)
1. A multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material is characterized in that the multi-dimensional cobaltosic oxide array is uniformly distributed on the surface of a biomass-derived porous carbon sheet, wherein the shape of a multi-dimensional cobaltosic oxide array unit is one of needle shape, sheet shape and sea urchin ball shape, and the biomass source of the porous carbon sheet is thousands of sheets.
2. The preparation method of the multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material as claimed in claim 1, characterized by comprising the following steps:
step 1, preparing a biomass-based porous carbon sheet material: cleaning, drying and calcining the biomass sheets under protective gas, and cooling to obtain the carbonized biomass;
step 2, preparing the multi-dimensional cobaltosic oxide array/biomass derived porous carbon sheet composite wave-absorbing material: dissolving cobalt nitrate hexahydrate, urea and ammonium fluoride in a certain proportion in deionized water, and magnetically stirring to obtain a pink transparent solution; immersing the porous carbon sheet prepared in the step 1 into the solution for hydrothermal reaction, and after the reaction is finished, performing suction filtration to obtain a light pink precursor; and finally, calcining the precursor in the air, and cooling to obtain a series of multi-dimensional cobaltosic oxide array/biomass-derived porous carbon sheet composite wave-absorbing materials.
3. The preparation method of the multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material as claimed in claim 2, wherein the heating rate of the calcination in the step 1 is 1-10 ℃/min, the calcination temperature is 600-800 ℃, the calcination time is 90-180 min, and the protective atmosphere is one or more selected from argon and nitrogen.
4. The preparation method of the multi-dimensional cobaltosic oxide array/biomass-based porous carbon sheet composite wave-absorbing material as claimed in claim 2, wherein the mass ratio of the porous carbon sheet to the cobaltous nitrate hexahydrate to the urea to the ammonium fluoride to the deionized water in step 2 is 1: (0.72-2.18): (0.75-2.25): (0.38-1.13): (100-300); the hydrothermal reaction temperature is 100-130 ℃, and the reaction time is 360-720 min; the calcination temperature is 300-450 ℃, and the calcination time is 120-240 min.
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CN115323766A (en) * | 2022-08-24 | 2022-11-11 | 安徽理工大学环境友好材料与职业健康研究院(芜湖) | Cobaltosic oxide/carbon cloth flexible wave-absorbing material and preparation method thereof |
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CN104263317A (en) * | 2014-09-26 | 2015-01-07 | 厦门大学 | Method for synthesizing cobalt oxide/graphene composite wave-absorbing material |
CN109494038A (en) * | 2018-11-06 | 2019-03-19 | 同济大学 | Ferroso-ferric oxide-nanoporous carbon nano-composite material and the preparation method and application thereof |
CN111019603A (en) * | 2019-11-20 | 2020-04-17 | 中车青岛四方机车车辆股份有限公司 | Cobaltosic oxide/carbon fiber composite material and preparation method and application thereof |
CN114068166A (en) * | 2021-11-09 | 2022-02-18 | 同济大学 | Hierarchical pore structure carbon-based magnetic composite material and preparation method and application thereof |
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CN104263317A (en) * | 2014-09-26 | 2015-01-07 | 厦门大学 | Method for synthesizing cobalt oxide/graphene composite wave-absorbing material |
CN109494038A (en) * | 2018-11-06 | 2019-03-19 | 同济大学 | Ferroso-ferric oxide-nanoporous carbon nano-composite material and the preparation method and application thereof |
CN111019603A (en) * | 2019-11-20 | 2020-04-17 | 中车青岛四方机车车辆股份有限公司 | Cobaltosic oxide/carbon fiber composite material and preparation method and application thereof |
CN114068166A (en) * | 2021-11-09 | 2022-02-18 | 同济大学 | Hierarchical pore structure carbon-based magnetic composite material and preparation method and application thereof |
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CN115323766A (en) * | 2022-08-24 | 2022-11-11 | 安徽理工大学环境友好材料与职业健康研究院(芜湖) | Cobaltosic oxide/carbon cloth flexible wave-absorbing material and preparation method thereof |
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