CN111269694A - Magnetoelectric composite nano porous wave-absorbing material and preparation method thereof - Google Patents
Magnetoelectric composite nano porous wave-absorbing material and preparation method thereof Download PDFInfo
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- 239000011358 absorbing material Substances 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 8
- FBHPRUXJQNWTEW-UHFFFAOYSA-N 1-benzyl-2-methylimidazole Chemical compound CC1=NC=CN1CC1=CC=CC=C1 FBHPRUXJQNWTEW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims abstract description 7
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims abstract description 6
- 229940011182 cobalt acetate Drugs 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000011148 porous material Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 230000005415 magnetization Effects 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 238000001354 calcination Methods 0.000 description 5
- 229910000428 cobalt oxide Inorganic materials 0.000 description 5
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 5
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000004685 tetrahydrates Chemical class 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
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- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
Abstract
The invention relates to a magnetoelectric composite nano porous wave-absorbing material and a preparation method thereof, wherein the wave-absorbing material comprises the following components in percentage by mass in the total amount of the wave-absorbing material: 15-45% of CoO, 10-40% of Co and 40-55% of porous carbon. Solid raw materials of dodecyl trimethyl ammonium bromide and Co (NO)3)2Mixing cobalt acetate and 1-benzyl-2-methylimidazole, dissolving in water, stirring, and standing to obtain a purple precursor mixed solution; centrifuging and collecting the purple centrifugation product; washed and dried to obtain Co (OH)2@ ZIF-67 complex precursor; the precursor is carbonized in a protective atmosphere to obtain the magnetoelectric composite nano porous wave-absorbing material which has larger reflection loss and absorption bandwidth and can be applied to human body electromagnetic wave protection and radar electromagnetic wave absorption coatings.
Description
Technical Field
The invention belongs to the technical field of functional materials, relates to a wave-absorbing material and a preparation method thereof, and particularly relates to a magnetoelectric composite nano porous wave-absorbing material and a preparation method thereof.
Background
With the more serious electromagnetic radiation pollution in the current society, the requirements of people on electromagnetic protection are more and more stringent. The light and high-efficiency electromagnetic wave absorption material can play an effective role in attenuating electromagnetic waves. However, it is often difficult to achieve the requirements of light weight, high efficiency and wide frequency with a single magnetic loss or dielectric loss material. Therefore, it is an effective method to solve this problem to prepare a composite absorbent having a synergistic effect of magnetic loss and dielectric loss. The magnetoelectric composite nano porous wave-absorbing material contains a large amount of mesoporous pores, so that electromagnetic wave energy can more easily enter the material. The dielectric loss of the material is mainly derived from the porous carbon. When electromagnetic waves are incident into the material, part of electrons can be accumulated on the mesoporous pore wall to form interface polarization, and the dielectric loss capacity of the material is enhanced through interface polarization relaxation loss.
Disclosure of Invention
The invention aims to provide a magnetoelectric composite nano porous wave-absorbing material for improving the defects of the prior art, which has larger reflection loss and absorption bandwidth; another object of the present invention is to provide a process for the preparation of the above-mentioned materials, which is simple, inexpensive in raw materials and good in reproducibility.
The technical scheme of the invention is as follows: aiming at the technical requirement that the wave-absorbing material needs to reach light weight, high efficiency and porosity, a nanometer needle-shaped precursor is introduced, and after carbonization, the magnetic oxide and nanometer porous carbon are compounded; firstly, the ZIF-67 derived porous carbon material has excellent wave absorbing performance, and in the invention, the ZIF-67 is tried to be respectively compounded with a material cobalt oxide phase with good magnetic loss characteristic, so that the magnetic loss capability of the MOFs derived porous carbon is further improved, and the electromagnetic loss composite wave absorbing material is obtained. CoO itself is also a good microwave absorber because of its high saturation magnetization, magnetic loss and large anisotropy field. Therefore, in the present invention, a magnetic oxide of CoO is selected to be combined with ZIF-67.
The specific technical scheme of the invention is as follows: a magnetoelectric composite nano porous wave-absorbing material is characterized in that the wave-absorbing material comprises the following components in percentage by mass in the total amount of the wave-absorbing material: 15-45% of CoO, 78-40% of Co10 and 40-55% of porous carbon.
The invention also provides a method for preparing the magnetoelectric composite nano porous wave-absorbing material, which comprises the following steps:
weighing solid raw materials according to the components and proportion of the solid raw materials, mixing, dissolving in water, stirring, and standing to obtain a purple precursor mixed solution;
(II) centrifuging the purple precursor mixed solution and collecting a purple centrifugal product; washing with deionized water, drying to obtain Co (OH)2@ ZIF-67 complex precursor;
(III) mixing Co with (OH)2And carbonizing the @ ZIF-67 compound precursor in a protective atmosphere at 500-600 ℃ for 2-3 hours.
The solid raw material components and the mass percentages of the components in the total amount of the solid raw materials are respectively as follows: dodecyl trimethyl ammonium bromide 1.4-3.6 wt% and Co (NO)3)2(Co (NO) is preferred3)2。6H23.6 to 4.4 percent of O), 18.5 to 21.2 percent of cobalt acetate (preferably cobalt acetate (II) tetrahydrate) and 73 to 74 percent of 1-benzyl-2-methylimidazole.
Preferably, the centrifugal rotating speed is 8000-10000 r/min; the centrifugation time is 3-5 min.
Preferably, the protective atmosphere is nitrogen, argon or helium.
The saturation magnetization intensity of the magnetoelectric composite nano porous wave-absorbing material prepared by the invention is 21.6-39.5 emu/g, the coercive force is 650-1200 Koe, and the specific surface area of a sample is 204-282 m2Per g, the total pore volume is 0.15-0.25 cm3/g。
When the thickness of the magnetoelectric composite nano porous wave-absorbing material is 1.5-2.5 mm, the minimum reflection loss is-33.93-31.81 dB, and the effective bandwidth reaches 3.72-5.8 GHz.
In the invention, needle-shaped Co (OH) is synthesized in situ2And carrying out carbonization on the/ZIF-67 precursor in nitrogen or argon or helium atmosphere to obtain the CoO/Co/porous carbon composite material. CoO and Co particles are embedded into the porous carbon, so that the magnetic loss capacity of the material is improved, the impedance matching of the material is optimized, and the nano particles show good microwave absorption performance. First, in situ synthesis of Co (OH)2And calcining the/ZIF-67 precursor in nitrogen or argon or helium atmosphere to obtain the CoO/Co/porous carbon material.
Has the advantages that:
the magnetoelectric composite nano porous wave-absorbing material prepared by the invention has larger reflection loss and absorption bandwidth; the preparation method is simple, the raw materials are cheap, and the repeatability is good.
Drawings
FIG. 1 is a graph of the reflection loss at different thicknesses of the product of cobalt oxide and ZIF-67 composite of example 1 at 500 deg.C;
FIG. 2 is a graph of the reflection loss at different thicknesses for the product of cobalt oxide and ZIF-67 composite of example 2 at 550 deg.C;
FIG. 3 graph of reflection loss of the cobalt oxide and ZIF-67 composite at 600 deg.C for different thicknesses of the resulting product of example 3;
FIG. 4 is a graph of the reflection loss of the product obtained from the cobalt oxide and ZIF-67 composite at 650 deg.C for different thicknesses.
Detailed Description
Example 1
Ten 0.06g of dialkyltrimethylammonium bromide, 0.18g of Co (NO)3)2·6H2O, 0.88g of cobalt (II) acetate tetrahydrate (98%) and 3.04g of 1-benzyl-2-methylimidazole are dissolved in 30ml of deionized water, and the mixed solution is stirred at room temperature for 5 hours and then stands for 24 hours to obtain a purple precursor mixed solution. The purple precursor mixed solution was centrifuged (10000r/min, 5min) and washed 3 times with deionized water. Drying the wet product in a vacuum drying oven at 80 ℃ for 2h, and then performing pyrolysis at 500 ℃ for 3h in a nitrogen atmosphere to obtain a CoO/Co/porous carbon composite wave-absorbing material; it is composed ofThe medium CoO accounts for 45%, the Co accounts for 15%, the porous carbon accounts for 40%, and as shown in FIG. 1, when the thickness is 1.5-2.5 mm, the minimum Reflection Loss (RL) is-32.48 dB, and the effective width is 3.72 GHz; as shown in Table I, the saturation magnetization is 21.6emu/g, and the coercivity is 960Koe, and the specific surface area of the sample is 204.97m2Per g, total pore volume of 0.1518cm3/g。
Example 2
0.14g of dodecyltrimethylammonium bromide, 0.144g of Co (NO)3)2·6H2O, 0.74g of cobalt (II) acetate tetrahydrate (98%) and 2.88g of 1-benzyl-2-methylimidazole are dissolved in 30ml of deionized water, the mixed solution is stirred for 5 hours at room temperature and then stands for 24 hours to obtain a purple precursor mixed solution, and the purple precursor mixed solution is subjected to centrifugal separation (10000r/min, 3min) and washed 3 times with deionized water. And drying the wet product in a vacuum drying oven at 80 ℃ for 2h, and then carrying out pyrolysis at 550 ℃ for 3h in a nitrogen atmosphere to obtain the CoO/Co/porous carbon composite wave-absorbing material. Wherein the CoO accounts for 35%, the Co accounts for 20%, the porous carbon accounts for 45%, as shown in FIG. 2, when the thickness is 1.5-2.5 mm, the minimum Reflection Loss (RL) is-33.93 dB, and the effective width is 5.8 GHz; as shown in Table I, the sample with the saturation magnetization of 24.8emu/g and the coercive force of 1220Koe has a specific surface area of 204.93m2Per g, total pore volume of 0.1831cm3/g。
Example 3
0.1g of dodecyltrimethylammonium bromide, 0.168g of Co (NO)3)2·6H2O, 0.8g of cobalt (II) acetate tetrahydrate (98 percent) and 2.92g of 1-benzyl-2-methylimidazole are dissolved in 30ml of deionized water, the mixed solution is stirred for 5 hours at room temperature and then stands for 24 hours to obtain a purple precursor mixed solution, and the purple precursor mixed solution is subjected to centrifugal separation (8000r/min, 5 minutes) and washed for 2 times by the deionized water. And drying the wet product in a vacuum drying oven at 70 ℃ for 3h, and then carrying out 600 ℃ pyrolysis for 2h in a nitrogen atmosphere to obtain the CoO/Co/porous carbon composite wave-absorbing material. Wherein CoO accounts for 20%, Co accounts for 33%, and porous carbon accounts for 47%, as shown in FIG. 3, when the thickness is 1.5-2.5 mm, the minimum Reflection Loss (RL) is-31.81 dB, and the effective width is 4.0 GHz; as shown in Table I, the saturation magnetization was 30.4emu/g, and the coercivity was set to beThe sample with a force of 650Koe had a specific surface area of 207.17m2Per g, total pore volume of 0.2362cm3/g。
Comparative example 1
0.12g of dodecyltrimethylammonium bromide, 0.16g of Co (NO)3)2·6H2O, 0.76g of cobalt (II) acetate tetrahydrate (98 percent) and 2.96g of 1-benzyl-2-methylimidazole are dissolved in 30ml of deionized water, the mixed solution is stirred for 5 hours at room temperature and then stands for 24 hours to obtain a purple precursor mixed solution, and the purple precursor mixed solution is subjected to centrifugal separation (10000r/min, 3min) and washed for 3 times by the deionized water. And drying the wet product in a vacuum drying oven at 80 ℃ for 2h, and then carrying out pyrolysis at 650 ℃ for 2h in a nitrogen atmosphere to obtain the CoO/Co/porous carbon composite wave-absorbing material. Wherein CoO accounts for 10%, Co accounts for 35%, and porous carbon accounts for 55%, as shown in FIG. 4, when the thickness is 1.5-2.5 mm, the magnetoelectric composite nano porous wave-absorbing material has no wave-absorbing performance; as shown in Table I, the sample had a saturation magnetization of 39.3emu/g and a coercivity of 700Koe and a specific surface area of 281.99m2Per g, total pore volume of 0.2479cm3/g。
When electromagnetic waves enter the wave-absorbing material, the energy of the electromagnetic waves is lost by generating oscillation current, and most of the electromagnetic waves are guided to enter the wave-absorbing material on the surface of the wave-absorbing material so as to reduce reflection.
And (3) testing electromagnetic parameters of products obtained at different calcining temperatures, and simulating the wave-absorbing performance of the products by calculation. The absorption bandwidths of the samples at a calcination temperature of 500, 550 and 600 ℃ were 3.72GHz, 5.80GHz and 4.0GHz, respectively, when the thickness was 2 mm. In these samples, the calcination temperature of 550 ℃ showed the best performance because of having closer values of dielectric loss and magnetic loss, i.e., having excellent impedance matching. In conclusion, the sample with the calcination temperature of 550 ℃ has the best wave-absorbing performance in all samples, when the thickness is only 2mm, the maximum reflection loss is-33.93 dB, and the effective absorption bandwidth can reach 5.8GHz (9.68 GHz-15.48 GHz). This is based on acicular Co (OH) as compared to the prepared pure ZIF-67 derived porous carbon material2The wave absorbing performance of the CoO/Co/porous carbon composite material of/ZIF-67 hasA greater lift.
The saturation magnetization, coercive force, specific surface area and total pore volume of the surface-magnetoelectric composite nano porous wave-absorbing material are shown.
Claims (6)
1. A magnetoelectric composite nano porous wave-absorbing material is characterized in that the wave-absorbing material comprises the following components in percentage by mass in the total amount of the wave-absorbing material: 15-45% of CoO, 10-40% of Co and 40-55% of porous carbon.
2. The method for preparing the magnetoelectric composite nano-porous wave-absorbing material according to claim 1 comprises the following specific steps:
according to the components of the solid raw materials and the mass percentage of each component in the total amount of the solid raw materials: dodecyl trimethyl ammonium bromide 1.4-3.6 wt% and Co (NO)3)23.6 to 4.4 percent of cobalt acetate, 18.5 to 21.2 percent of cobalt acetate and 73 to 74 percent of 1-benzyl-2-methylimidazole, weighing solid raw materials, mixing, dissolving in water, stirring, and standing to obtain a purple precursor mixed solution;
(II) centrifuging the purple precursor mixed solution and collecting a purple centrifugal product; washing with deionized water and drying to obtain Co (OH)2@ ZIF-67 complex precursor;
(III) mixing Co with (OH)2And carbonizing the @ ZIF-67 compound precursor in a protective atmosphere at 500-600 ℃ for 2-3 hours.
3. The method according to claim 2, wherein the centrifugal rotation speed is 8000 to 10000 r/min; the centrifugation time is 3-5 min.
4. The method of claim 2, wherein the protective atmosphere is nitrogen, argon or helium.
5. The method according to claim 2, wherein the saturation magnetization of the prepared magnetoelectric composite nano porous wave-absorbing material is 21.6-39.5 emu/g, the coercive force is 650-1200 Koe, and the specific surface area of the sample is 204-282 m2Per g, the total pore volume is 0.15-0.25 cm3/g。
6. The method according to claim 2, wherein the magnetoelectric composite nano porous wave-absorbing material has a minimum reflection loss of-33.93 to-31.81 dB and an effective bandwidth of 3.72 to 5.8GHz when the thickness is 1.5 to 2.5 mm.
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CN113511640A (en) * | 2021-05-26 | 2021-10-19 | 中国人民解放军国防科技大学 | Metal nanocrystalline-amorphous carbon composite wave-absorbing particle and preparation method thereof |
CN113801631A (en) * | 2021-11-09 | 2021-12-17 | 西北大学 | MnCo2O4@ ZIF-67/Ni wave-absorbing material and preparation method thereof |
CN115141031A (en) * | 2022-05-18 | 2022-10-04 | 安徽大学 | Electromagnetic wave absorption composite material and preparation method and application thereof |
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