CN113462356B - Preparation method of binary composite wave-absorbing material - Google Patents

Preparation method of binary composite wave-absorbing material Download PDF

Info

Publication number
CN113462356B
CN113462356B CN202110666165.2A CN202110666165A CN113462356B CN 113462356 B CN113462356 B CN 113462356B CN 202110666165 A CN202110666165 A CN 202110666165A CN 113462356 B CN113462356 B CN 113462356B
Authority
CN
China
Prior art keywords
nitrogen
porous carbon
doped porous
absorbing material
binary composite
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110666165.2A
Other languages
Chinese (zh)
Other versions
CN113462356A (en
Inventor
罗驹华
江陈烨
冯萌娜
贺盟
翟雪松
王旭
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yancheng Institute of Technology
Original Assignee
Yancheng Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yancheng Institute of Technology filed Critical Yancheng Institute of Technology
Priority to CN202110666165.2A priority Critical patent/CN113462356B/en
Publication of CN113462356A publication Critical patent/CN113462356A/en
Application granted granted Critical
Publication of CN113462356B publication Critical patent/CN113462356B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention relates to a preparation method of a binary composite wave-absorbing material, which comprises the steps of firstly preparing a ZIF-8 precursor, then placing the ZIF-8 precursor into a tube furnace, heating to 800-900 ℃ under a nitrogen atmosphere, preserving heat for 1-5 h, then cooling to room temperature to obtain nitrogen-doped porous carbon, adding the nitrogen-doped porous carbon into distilled water, stirring uniformly to obtain nitrogen-doped porous carbon suspension, sequentially adding sodium molybdate and thiourea into the nitrogen-doped porous carbon suspension, stirring uniformly, transferring the mixed solution into a reaction kettle, placing the reaction kettle into a drying oven, preserving heat for 12-36 h at 190-220 ℃, taking out the reaction kettle, naturally cooling at room temperature, carrying out suction filtration on the reaction solution, washing a solid product, and then carrying out vacuum drying to constant weight to obtain the binary composite wave-absorbing material. The method has the advantages of simple preparation flow, easy control and low production cost, and the prepared wave-absorbing material has the advantages of low density, wide wave-absorbing frequency and excellent wave-absorbing performance.

Description

Preparation method of binary composite wave-absorbing material
Technical Field
The invention belongs to the technical field of wave-absorbing materials, and particularly relates to a preparation method of a nitrogen-doped porous carbon/molybdenum disulfide binary composite wave-absorbing material.
Background
With the advent of the 5G age, electronic products are rapidly updated, and a certain amount of electromagnetic radiation is released in the use process of the electronic products, so that electromagnetic pollution is generated for a long time. Prolonged exposure to electromagnetic radiation can lead to reduced immunity and increased morbidity. Therefore, research into an absorbing material for preventing and eliminating electromagnetic waves has been focused on by researchers.
The material has the wave absorbing effect and needs to meet two conditions: impedance matching and attenuation matching. However, it is generally difficult to satisfy impedance matching for a single material, so it is often considered to perform multiple compounding or form a special structure on different dielectric materials to obtain a suitable impedance matching, so that more electromagnetic waves can smoothly enter the material to be attenuated. In addition, with the development of the wave-absorbing material, the 'thin, light, wide and strong' is four requirements of future research of the material, and the traditional wave-absorbing material such as a carbon-based material has strong wave-absorbing performance, but has narrow frequency band, so that the application of the wave-absorbing material in a wider range is limited to a certain extent.
Disclosure of Invention
The invention aims to solve the problems of high density and narrow wave-absorbing frequency band of the wave-absorbing material in the prior art, and provides a preparation method of a binary composite wave-absorbing material, which has the advantages of simple preparation flow, easy control and low production cost, and the prepared wave-absorbing material has the advantages of low density, wide wave-absorbing frequency band and excellent wave-absorbing performance.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a binary composite wave-absorbing material comprises the following steps:
(1) Respectively adding 2-methylimidazole and zinc nitrate hexahydrate into methanol, stirring and dissolving at room temperature to obtain a zinc nitrate solution and a 2-methylimidazole solution, dropwise adding the zinc nitrate solution into the 2-methylimidazole solution, continuously stirring for 30-60 min, aging for 12-36 h at room temperature, filtering the reaction solution, washing filter residues with ethanol, and vacuum drying the filter residues to constant weight to obtain a ZIF-8 precursor;
(2) Putting the ZIF-8 precursor prepared in the step (1) into a tube furnace, heating to 800-900 ℃ in nitrogen atmosphere, preserving heat for 1-5 h, and then cooling to room temperature to obtain nitrogen-doped porous carbon;
(3) Adding nitrogen-doped porous carbon into distilled water, stirring uniformly to obtain nitrogen-doped porous carbon suspension, sequentially adding sodium molybdate and thiourea into the nitrogen-doped porous carbon suspension, and stirring uniformly to obtain a mixed solution;
(4) And (3) transferring the mixed solution to a reaction kettle, placing the reaction kettle in a drying oven, preserving heat for 12-36 h at 190-220 ℃, taking out the reaction kettle, naturally cooling the reaction kettle at room temperature, carrying out suction filtration on the reaction solution, washing the solid product, and then carrying out vacuum drying to constant weight to obtain the binary composite wave-absorbing material.
Further, in the step (1), the molar ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 1: (7-10).
Further, in the step (1), the drying temperature is 50-80 ℃.
Further, in the step (2), the heating rate is 2-4 ℃/min.
Further, in the step (3), the molar ratio of the sodium molybdate to the nitrogen-doped porous carbon is 1 (6 to 15).
Further, in the step (4), the temperature of the vacuum drying is 50-80 ℃.
The invention has the beneficial effects that: according to the invention, the nitrogen-doped porous carbon is compounded with molybdenum disulfide by utilizing the characteristics of good microwave absorption performance of the nitrogen-doped porous carbon at low frequency, good thermal stability, strong chemical stability and the like, so that the impedance matching of the material can be effectively improved, and more electromagnetic waves are promoted to enter the material; in addition, the nitrogen doped porous carbon and molybdenum disulfide have stronger interface combination, so that the effective wave-absorbing frequency band can be widened, and the wave-absorbing performance can be enhanced.
Drawings
FIG. 1 is an XRD pattern of the binary composite wave-absorbing material prepared in example 1;
FIG. 2 is an SEM image of a binary composite wave-absorbing material prepared in example 1;
FIG. 3 is a graph showing the wave-absorbing performance of the binary composite wave-absorbing material prepared in example 1.
Detailed Description
The present invention will be specifically described with reference to examples below in order to make the objects and advantages of the present invention more apparent. It should be understood that the following text is intended to describe only one or more specific embodiments of the invention and does not limit the scope of the invention strictly as claimed.
Example 1
A preparation method of a binary composite wave-absorbing material comprises the following steps:
(1) Adding 6.849g of 2-methylimidazole and 2.933g of zinc nitrate hexahydrate into 100mL of methanol respectively, stirring and dissolving at room temperature to obtain zinc nitrate solution and 2-methylimidazole solution, dropwise adding the zinc nitrate solution into the 2-methylimidazole solution, continuously stirring for 40min, aging at room temperature for 24h, filtering the reaction solution, washing filter residues with ethanol, and drying the filter residues in a vacuum drying oven at 70 ℃ for 12h to obtain a ZIF-8 precursor;
(2) Grinding the ZIF-8 precursor prepared in the step (1) into fine powder, then placing the fine powder into a tube furnace, heating to 800 ℃ at a heating rate of 2 ℃/min under a nitrogen atmosphere, preserving heat for 3 hours, and then cooling to room temperature to obtain nitrogen-doped porous carbon;
(3) Adding 0.64g of nitrogen-doped porous carbon into 40mL of distilled water, uniformly stirring to obtain nitrogen-doped porous carbon suspension, sequentially adding 0.9677g of sodium molybdate and 1.1418g of thiourea into the nitrogen-doped porous carbon suspension, and uniformly stirring to obtain a mixed solution;
(4) And (3) transferring the mixed solution to a reaction kettle, placing the reaction kettle in a drying oven, preserving heat at 200 ℃ for 24 hours, taking out the reaction kettle, naturally cooling at room temperature, carrying out suction filtration on the reaction solution, washing the solid product, and then carrying out vacuum drying at 60 ℃ for 12 hours to obtain the binary composite wave-absorbing material.
Performing phase structure analysis on the obtained sample by using an X-ray diffractometer (XRD) and a Fourier transform infrared spectrometer (FTIR); the microstructure of the sample is analyzed by a Scanning Electron Microscope (SEM), a Transmission Electron Microscope (TEM) and a corresponding Mapping graph, and electromagnetic parameters of the sample are analyzed by a Vector Network Analyzer (VNA), so that the wave absorbing performance of the sample is calculated. The test results are shown in FIGS. 1-3.
FIG. 1 is a nitrogen doped porous carbon/molybdenum disulfide (NPC/MoS) prepared in example 1 2 ) The XRD pattern of the binary composite wave-absorbing material is shown in the figure 1 (a), which is the XRD pattern of the ZIF-8, and the ZIF-8 can be found to have a plurality of diffraction peaks and sharp peaks, which indicates that the ZIF-8 precursor is successfully prepared in the experimental process; FIG. 1 (b) is a calcined nitrogen-doped porous carbon material from which it can be seen that the diffraction peak attributed to the ZIF-8 precursor disappeared, leaving only a broad diffraction peak around 2θ=25°, indicating that ZIF-8 has been completely converted to a nitrogen-doped porous carbon (NPC) material; FIG. 1 (c) is molybdenum disulfide (MoS 2 ) The XRD pattern of the (B) is compared with the corresponding standard card, and the peak positions are basically consistent; FIG. 1 (d) is a nitrogen doped porous carbon/molybdenum disulfide (NPC/MoS) 2 ) The diffraction peak of molybdenum disulfide is evident from the figure, whereas the diffraction peak of nitrogen-doped porous carbon is not evident, probably due to the diffraction of nitrogen-doped porous carbonThe intensity of the peak is weaker and is masked by the diffraction peak of molybdenum disulfide.
FIG. 2 is a nitrogen doped porous carbon/molybdenum disulfide (NPC/MoS) prepared in example 1 2 ) SEM image of binary composite wave-absorbing material. In FIG. 2, (a-1) and (a-2), (b-1) and (b-2), (c-1) and (c-2), (d-1) and (d-2) are ZIF-8 precursors, NPC, moS, respectively 2 And NPC/MoS 2 According to the SEM image of the (2), the ZIF-8 precursor is rhombic dodecahedron, the grain size is about 500nm, the calcined porous carbon material still maintains the shape of the rhombic dodecahedron, but the surface is slightly concave, the size is slightly contracted, the molybdenum disulfide is spherical, and the size is between 3 and 4 mu m; as can be clearly seen from FIGS. 2 (d-1) and (d-2), the nitrogen doped porous carbon material is inlaid on the surface of molybdenum disulfide.
FIG. 3 is a nitrogen doped porous carbon/molybdenum disulfide (NPC/MoS) prepared in example 1 2 ) And the reflectivity loss curve of the binary composite wave absorbing material is 1.0-5.5 mm thick. From the graph, it can be found that the minimum reflection loss value is-34.9 dB when the thickness is 3.0mm and the frequency is 12GHz, and the effective absorption frequency bands are 6.2GHz respectively.
While the embodiments of the present invention have been described in detail with reference to the examples, the present invention is not limited to the above embodiments, and it will be apparent to those skilled in the art that various equivalent changes and substitutions can be made therein without departing from the principles of the present invention, and such equivalent changes and substitutions should also be considered to be within the scope of the present invention.

Claims (5)

1. The preparation method of the binary composite wave-absorbing material is characterized by comprising the following steps of:
(1) Respectively adding 2-methylimidazole and zinc nitrate hexahydrate into methanol, stirring and dissolving at room temperature to obtain a zinc nitrate solution and a 2-methylimidazole solution, dropwise adding the zinc nitrate solution into the 2-methylimidazole solution, continuously stirring for 30-60 min, aging for 12-36 h at room temperature, filtering the reaction solution, washing filter residues with ethanol, and vacuum drying the filter residues to constant weight to obtain a ZIF-8 precursor;
(2) Grinding the ZIF-8 precursor prepared in the step (1) into fine powder, then placing the fine powder into a tube furnace, heating to 800-900 ℃ in a nitrogen atmosphere, preserving heat for 1-5 h, and then cooling to room temperature to obtain nitrogen-doped porous carbon;
(3) Adding nitrogen-doped porous carbon into distilled water, stirring uniformly to obtain nitrogen-doped porous carbon suspension, sequentially adding sodium molybdate and thiourea into the nitrogen-doped porous carbon suspension, and stirring uniformly to obtain a mixed solution;
(4) Transferring the mixed solution to a reaction kettle and placing the reaction kettle in a drying oven, preserving heat for 12-36 hours at 190-220 ℃, taking out the reaction kettle, naturally cooling the reaction kettle at room temperature, carrying out suction filtration on the reaction solution, washing a solid product, and then carrying out vacuum drying to constant weight to obtain a binary composite wave-absorbing material nitrogen-doped porous carbon/molybdenum disulfide, wherein the molybdenum disulfide is spherical, the size is 3-4 mu m, and the nitrogen-doped porous carbon material is embedded on the surface of the molybdenum disulfide;
in the step (3), the molar ratio of the sodium molybdate to the nitrogen-doped porous carbon is 1 (6-15).
2. The method for preparing a binary composite wave-absorbing material according to claim 1, wherein in the step (1), the molar ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 1: (7-10).
3. The method for producing a binary composite wave-absorbing material according to claim 1, wherein in the step (1), the drying temperature is 50 to 80 ℃.
4. The method for preparing a binary composite wave-absorbing material according to claim 1, wherein in the step (2), the heating rate is 2-4 ℃/min.
5. The method of producing a binary composite absorbing material according to any one of claims 1 to 4, wherein in the step (4), the temperature of the vacuum drying is 50 to 80 ℃.
CN202110666165.2A 2021-06-16 2021-06-16 Preparation method of binary composite wave-absorbing material Active CN113462356B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110666165.2A CN113462356B (en) 2021-06-16 2021-06-16 Preparation method of binary composite wave-absorbing material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110666165.2A CN113462356B (en) 2021-06-16 2021-06-16 Preparation method of binary composite wave-absorbing material

Publications (2)

Publication Number Publication Date
CN113462356A CN113462356A (en) 2021-10-01
CN113462356B true CN113462356B (en) 2023-11-28

Family

ID=77870253

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110666165.2A Active CN113462356B (en) 2021-06-16 2021-06-16 Preparation method of binary composite wave-absorbing material

Country Status (1)

Country Link
CN (1) CN113462356B (en)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109607510A (en) * 2019-01-15 2019-04-12 广西大学 ZIF base nitrogen-doped porous carbon material and preparation method thereof
CN109786682A (en) * 2018-06-20 2019-05-21 信阳师范学院 12 face nucleome anode material of lithium-ion battery of a kind of two selenizing molybdenum@nitrogen-doped carbon and preparation method thereof, sodium-ion battery
CN110492083A (en) * 2019-08-28 2019-11-22 青岛大学 A kind of preparation method of molybdenum disulfide/graphene/carbon multistage hole composite material
CN110787814A (en) * 2019-11-07 2020-02-14 汕头大学 Layered hollow ZnCdS/MoS2Heterojunction cage and preparation and application thereof
CN112063365A (en) * 2020-09-04 2020-12-11 山东大学 Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof
CN112916861A (en) * 2021-01-20 2021-06-08 昆明理工大学 Fe2Mo/NC binary alloy nano catalyst and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109786682A (en) * 2018-06-20 2019-05-21 信阳师范学院 12 face nucleome anode material of lithium-ion battery of a kind of two selenizing molybdenum@nitrogen-doped carbon and preparation method thereof, sodium-ion battery
CN109607510A (en) * 2019-01-15 2019-04-12 广西大学 ZIF base nitrogen-doped porous carbon material and preparation method thereof
CN110492083A (en) * 2019-08-28 2019-11-22 青岛大学 A kind of preparation method of molybdenum disulfide/graphene/carbon multistage hole composite material
CN110787814A (en) * 2019-11-07 2020-02-14 汕头大学 Layered hollow ZnCdS/MoS2Heterojunction cage and preparation and application thereof
CN112063365A (en) * 2020-09-04 2020-12-11 山东大学 Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof
CN112916861A (en) * 2021-01-20 2021-06-08 昆明理工大学 Fe2Mo/NC binary alloy nano catalyst and preparation method thereof

Also Published As

Publication number Publication date
CN113462356A (en) 2021-10-01

Similar Documents

Publication Publication Date Title
CN112961650A (en) Tri-metal organic framework derived iron-nickel alloy/porous carbon ultrathin wave absorber and preparation method thereof
CN114195197B (en) Magnetic porous carbon compound and preparation method and application thereof
CN112047386A (en) Heating modified MXene/ferroferric oxide composite wave-absorbing material and preparation method thereof
CN112752496B (en) Hollow nitrogen-doped nickel oxide/nickel/carbon composite material, preparation method and application
CN111818785B (en) Low-temperature foaming process for preparing thin-layer carbon-loaded nano ZnO wave-absorbing material in batches
CN113825380A (en) Cobalt/manganese oxide/porous graphitized carbon wave-absorbing material and preparation method thereof
CN110746931B (en) Method for preparing ITO/porous carbon composite wave-absorbing material by taking In-MOFs as template
CN113735093A (en) Porous N-doped Co @ C composite material and preparation method and application thereof
CN113462356B (en) Preparation method of binary composite wave-absorbing material
CN113429933A (en) Ferroferric oxide/biomass porous carbon composite wave-absorbing material and preparation method thereof
CN112920774A (en) Hexagonal Co @ C wave absorber, preparation method and application
CN115332821A (en) Preparation method of CoNi/NC wave-absorbing material
CN115745627A (en) SiCN ceramic wave absorbing agent and preparation method thereof
CN115318210A (en) Preparation method and application of cobalt disulfide/porous carbon/silicon carbide aerogel composite material for electromagnetic shielding
CN114455630A (en) Multi-band composite electromagnetic wave absorption material and preparation method and application thereof
CN114614272A (en) MXene/Co/C composite wave-absorbing material derived from MOF and preparation method thereof
CN114206091A (en) CoFe/C-CNT wave-absorbing material and preparation process and application thereof
CN114314679A (en) Polypyrrole-coated ferroferric oxide nanoflower wave-absorbing material, preparation method and application
CN115340131B (en) Preparation method of cobalt disulfide-polythiophene wave-absorbing material
CN114875391B (en) Preparation method of FeCo alloy coated foam nickel wave-absorbing material
CN115926182B (en) Preparation method of novel braided Ni-MOF wave-absorbing material
CN117511501B (en) Composite wave-absorbing material with core-shell structure and preparation method thereof
CN116656317A (en) MoS (MoS) 2 /Ti 2 CT x MXene composite wave-absorbing material and preparation method thereof
CN113708086B (en) Transition metal nano powder/carbon nano tube composite material and preparation method and application thereof
CN118308068A (en) Preparation method and application of multidimensional assembled hollow MOF derivative/molybdenum disulfide composite material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
EE01 Entry into force of recordation of patent licensing contract
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20211001

Assignee: DONGTAI GAOKE TECHNOLOGY INNOVATION PARK Co.,Ltd.

Assignor: YANCHENG INSTITUTE OF TECHNOLOGY

Contract record no.: X2024980001369

Denomination of invention: Preparation method of a binary composite absorbing material

Granted publication date: 20231128

License type: Common License

Record date: 20240124

EC01 Cancellation of recordation of patent licensing contract
EC01 Cancellation of recordation of patent licensing contract

Assignee: DONGTAI GAOKE TECHNOLOGY INNOVATION PARK Co.,Ltd.

Assignor: YANCHENG INSTITUTE OF TECHNOLOGY

Contract record no.: X2024980001369

Date of cancellation: 20240407